CN107973559A - The preparation method and applications of porous geological polymer microballoon - Google Patents
The preparation method and applications of porous geological polymer microballoon Download PDFInfo
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- CN107973559A CN107973559A CN201711177741.7A CN201711177741A CN107973559A CN 107973559 A CN107973559 A CN 107973559A CN 201711177741 A CN201711177741 A CN 201711177741A CN 107973559 A CN107973559 A CN 107973559A
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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
- C04B28/006—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 mineral polymers, e.g. geopolymers of the Davidovits type
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
- C02F2101/006—Radioactive compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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Abstract
The invention discloses a kind of preparation method of porous geological polymer microballoon, and porous geological polymer microballoon is made using scattered suspension solidification method.Compared with prior art, the present invention cures without high-temperature calcination, it is not required that adds other auxiliary agents, but realizes low-temperature setting, one-pass molding granulation.Meanwhile The invention also achieves a large amount of uses of solid waste, and raw material sources are extensive, and of low cost, technique is simple, and whole process is nontoxic and pollution-free.In addition, to prepare porous geological polymer microballoon efficient by the present invention, into sphericity more than 90%；Particle size is adjustable, even aperture distribution；Pore volume is larger, controllable, and microballoon specific surface area reaches 110m2/ g, can be directly used for the packed column of post separation.Experiment shows that porous geological polymer microballoon of the invention works well heavy metal adsorption, can be used as heavy metal absorbent, and application prospect is extensive in terms of heavy metal in going water removal and radioactive element.
Description
Technical field
The invention belongs to adsorbing agent carrier technical field, more particularly to a kind of preparation method of porous geological polymer microballoon
And its application.
Background technology
Post separation method is a kind of effective ways of heavy metal and radioactive element in water removal, and partial adsorbates material is as zeolite
Molecular sieve, activated carbon, can directly carry out filling out column, but for organic solvent or the less inorganic adsorbing material of particle diameter, it is necessary to
Being supported could use on the spherical particle carrier of appropriate particle diameter.At present, silica gel, polymer-based composite and macropore silicon
Sill is exploited, and improves the use scope of post separation method.However, its complex production process, cost is higher, limits
Its industrial applications.
Geo-polymer is a kind of raw material (including natural products, artificial synthesized powder and work by containing alumino-silicate
Industry discarded object etc.), excitation is carried out so that preparing has [AlO by acid or alkaline matter under room temperature or hot conditions4] and
[SiO4] tetrahedral three-dimensional network inorganic coagulation material.Geo-polymer compares other inorganic polymers, have excellent performance,
Preparation process is simple, energy consumption is low, advantages of environment protection, can be widely applied to construction material, nuclear waste disposal, casting, metallurgy,
The fields such as refractory material, plastics.At present, the method that porous, inorganic microballoon mainly uses high-temperature calcination is prepared both at home and abroad, is prepared
Journey is cumbersome, and cost is higher.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of simple, cheap, environmental protection porous geological polymer microballoon
Preparation method and applications.
In order to solve the above technical problems, the present invention uses following technical scheme：
The preparation method of porous geological polymer microballoon, using scattered suspension solidification method, is specifically carried out by following operation：Will
Powder and aqueous slkali with alkali-activated carbonatite activity are mixed evenly as mixed slurry, then by finely dispersed pore creating material water
Solution is slowly added to continue to stir in mixed slurry, and the slurry stirred evenly is finally added dropwise to the hot dimethyl-silicon of high speed dispersion
In oil, then conserve through baking oven, the synthetic product after maintenance is poured out from dimethicone, is filtered, is calcined, to obtain the final product.
Powder with alkali-activated carbonatite activity is slag, slag, grain slag, flyash, silicon ash point, silicon powder, red mud, higher ridge
Soil, synthetic powder.
Aqueous slkali is sodium silicate, potassium water glass, sodium hydroxide, potassium hydroxide, lithium hydroxide, strontium hydroxide, hydroxide
Caesium, carbonate, bicarbonate, sulfate, disulfate, aluminate, the solution of aluminosilicate.
Pore creating material for calcium carbonate, ammonium hydrogen carbonate, sodium acid carbonate, polyethylene glycol, polymethyl methacrylate, polyvinyl chloride,
Polyvinyl alcohol, sodium alginate, polystyrene.
The preparation method of above-mentioned porous geological polymer microballoon, comprises the following steps：
(1) prepared by slurry：Powder with alkali-activated carbonatite activity and aqueous slkali are mixed evenly as mixed slurry, so
Afterwards finely dispersed pore creating material aqueous solution is slowly added to continue to stir in mixed slurry, be uniformly mixed, mixing speed 500-
4000 revs/min, stir 1-5 minutes, system is become homogeneous slurry；
(2) balling-up：The homogeneous slurry of step (1) is added dropwise in the hot dimethicone of high speed dispersion；
(3) cure：The dimethicone of step (2) and products therefrom are put into togerther in baking oven carry out it is curing；
(4) filter：The dimethicone of step (3) and its products therefrom are subjected to vacuum filter, obtain geo-polymer
Microballoon；
(5) calcine：The geo-polymer microballoon of step (4) is calcined in Muffle furnace, it is micro- up to porous geological polymer
Ball.
In step (1) with alkali-activated carbonatite activity powder in terms of slag, aqueous slkali in terms of sodium silicate, solvent in terms of water,
For pore creating material in terms of polymethyl methacrylate, its mass ratio is slag: sodium silicate: water: polymethyl methacrylate=1:
0.1-1∶0.1-0.7∶0-0.005。
The temperature of hot dimethicone is 40-150 degrees Celsius in step (2), and mixing speed is 200-2000 revs/min；
In step (3) temperature of baking oven be 50-150 degrees Celsius, the curing time for 5 minutes -48 it is small when；
The temperature of calcining is 200-900 degrees Celsius in step (5), when calcination time is 0.5-12 small.
Porous geological polymer microballoon obtained above is used as adsorbent.
Porous geological polymer microballoon obtained above is used as heavy metal or radioactive element adsorbent.
The particle mean size of porous geological polymer microballoon is 5-500 microns, porosity 10-60%, specific surface area 20-
120m2/g。
For existing porous, inorganic microballoon and its prepare there are the problem of, inventor establishes a kind of porous geological polymer
The preparation method of microballoon, using scattered suspension solidification method, is specifically carried out by following operation：By the powder with alkali-activated carbonatite activity and
Aqueous slkali is mixed evenly as mixed slurry, and then finely dispersed pore creating material aqueous solution is slowly added in mixed slurry
Continue to stir, finally the slurry stirred evenly is added dropwise in the hot dimethicone of high speed dispersion, then conserved through baking oven, conserved
Synthetic product afterwards is poured out from dimethicone, is filtered, is calcined, to obtain the final product.Compared with prior art, the present invention is forged without high temperature
Baking, it is not required that add other auxiliary agents, but realize low-temperature setting, one-pass molding granulation.Meanwhile the present invention also realizes
A large amount of uses of solid waste, and raw material sources are extensive, and of low cost, technique is simple, whole process is nontoxic and pollution-free.In addition,
It is efficient that the present invention prepares porous geological polymer microballoon, into sphericity more than 90%；Particle size is adjustable, even aperture distribution；
Pore volume is larger, controllable, and microballoon specific surface area reaches 110m2/ g, can be directly used for the packed column of post separation.Experiment shows,
The porous geological polymer microballoon of the present invention is good to heavy metal and radioactive element adsorption effect, can be used as heavy metal adsorption
Agent, application prospect is extensive in terms of heavy metal in going water removal and radioactive element.
Brief description of the drawings
Fig. 1 is the light microscope microphoto using porous geological polymer microballoon made from preparation method of the present invention
(50 times).
Fig. 2 is the scanning electron microscope microphoto using porous geological polymer microballoon made from preparation method of the present invention
(1000 times).
Fig. 3 is the scanning electron microscope microphoto using porous geological polymer microballoon made from preparation method of the present invention
(2000 times).
Embodiment
Embodiment 1
(1) prepared by slurry：30g slags and 12g liquid sodium silicates (modulus 2.5) are mixed evenly as mixing slurry
Material, finely dispersed pore creating material aqueous solution (3g calcium carbonate+5g water) then be slowly added to continue to stir in mixed slurry, is mixed
Uniformly, mixing speed is 500 revs/min, stirs 2 minutes, system is become homogeneous slurry；
(2) balling-up：The homogeneous slurry of step (1) is added dropwise in the hot dimethicone of high speed dispersion, temperature is taken the photograph for 50
Family name's degree, mixing speed are 200 revs/min；
(3) cure：The dimethicone of step (2) and products therefrom are put into togerther in baking oven and carry out curing, temperature
Spend for 60 degrees Celsius, when the curing time is 1 small；
(4) filter：The dimethicone of step (3) and its products therefrom are subjected to vacuum filter, obtain geo-polymer
Microballoon；
(5) calcine：The geo-polymer microballoon of step (4) is calcined in Muffle furnace, temperature is 700 degrees Celsius, calcining
When time is 12 small, up to porous geological polymer.
After testing, 5-300 μm of microspherulite diameter, pore volume 0.1998cm3/ g, specific surface area 35.36m2/g。
The porous geological polymer obtained by 0.06g is weighed in the Pb that 100mL concentration is 150ppm2+In solution 24 it is small when, inhale
Attached amount is 268.7mg/g.
Embodiment 2
(1) prepared by slurry：20g slags and 8.57g liquid sodium silicates (modulus 1.5) are mixed evenly as mixing slurry
Material, finely dispersed pore creating material aqueous solution (10g calcium carbonate+10g water) then be slowly added to continue to stir in mixed slurry, is mixed
Close uniformly, mixing speed is 1000 revs/min, stirs 1 minute, system is become homogeneous slurry；
(2) balling-up：The homogeneous slurry of step (1) is added dropwise in the hot dimethicone of high speed dispersion, temperature is taken the photograph for 100
Family name's degree, mixing speed are 500 revs/min；
(3) cure：The dimethicone of step (2) and products therefrom are put into togerther in baking oven and carry out curing, temperature
Spend for 70 degrees Celsius, when the curing time is 12 small；
(4) filter：The dimethicone of step (3) and its products therefrom are subjected to vacuum filter, obtain geo-polymer
Microballoon；
(5) calcine：The geo-polymer microballoon of step (4) is calcined in Muffle furnace, temperature is 500 degrees Celsius, calcining
When time is 12 small, up to porous geological polymer.
After testing, 50-500 μm of microspherulite diameter, pore volume 0.2498cm3/ g, specific surface area 65.48m2/g。
The porous geological polymer obtained by 0.08g is weighed in the Pb that 100mL concentration is 300ppm2+In solution 36 it is small when, inhale
Attached amount is 301.5mg/g.
Embodiment 3
(1) prepared by slurry：20g metakaolins, 10g slags and 12g sodium hydroxide solutions (10 moles of concentration) are mixed and stirred
Mixing uniformly becomes mixed slurry, then that finely dispersed pore creating material aqueous solution (2g polymethyl methacrylate+25g water) is slow
Add in mixed slurry and continue to stir, be uniformly mixed, mixing speed is 300 revs/min, is stirred 5 minutes, system is become homogeneous
Slurry；
(2) balling-up：The homogeneous slurry of step (1) is added dropwise in the hot dimethicone of high speed dispersion, temperature is taken the photograph for 90
Family name's degree, mixing speed are 700 revs/min；
(3) cure：The dimethicone of step (2) and products therefrom are put into togerther in baking oven and carry out curing, temperature
Spend for 90 degrees Celsius, when the curing time is 1 small；
(4) filter：The dimethicone of step (3) and its products therefrom are subjected to vacuum filter, obtain geo-polymer
Microballoon；
(5) calcine：The geo-polymer microballoon of step (4) is calcined in Muffle furnace, temperature is 800 degrees Celsius, calcining
When time is 12 small, up to porous geological polymer.
After testing, 10-300 μm of microspherulite diameter, pore volume 0.1836cm3/ g, specific surface area 28.75m2/g。
The porous geological polymer obtained by 0.06g is weighed in the Sr that 30mL concentration is 50ppm2+In solution 1 it is small when, adsorbance
For 30.65mg/g.
Embodiment 4
(1) prepared by slurry：30g metakaolins and 20g sodium hydroxide solutions (8 moles of concentration), which are mixed evenly, to be become
Mixed slurry, finely dispersed pore creating material aqueous solution (10g polymethyl methacrylate+15g water) then be slowly added to mix
Continue to stir in slurry, be uniformly mixed, mixing speed is 1200 revs/min, stirs 1 minute, system is become homogeneous slurry；
(2) balling-up：The homogeneous slurry of step (1) is added dropwise in the hot dimethicone of high speed dispersion, temperature is taken the photograph for 40
Family name's degree, mixing speed are 200 revs/min；
(3) cure：The dimethicone of step (2) and products therefrom are put into togerther in baking oven and carry out curing, temperature
Spend for 60 degrees Celsius, when the curing time is 2 small；
(4) filter：The dimethicone of step (3) and its products therefrom are subjected to vacuum filter, obtain geo-polymer
Microballoon；
(5) calcine：The geo-polymer microballoon of step (4) is calcined in Muffle furnace, temperature is 400 degrees Celsius, calcining
When time is 12 small, up to porous geological polymer.
After testing, 20-400 μm of microspherulite diameter, pore volume 0.2798cm3/ g, specific surface area 100.56m2/g。
The porous geological polymer obtained by 0.06g is weighed in the Sr that 30mL concentration is 150ppm2+In solution 2 it is small when, absorption
Measure as 50.54mg/g.
Claims (10)
- A kind of 1. preparation method of porous geological polymer microballoon, it is characterised in that using scattered suspension solidification method, it is specific press with Lower operation carries out：Powder with alkali-activated carbonatite activity and aqueous slkali are mixed evenly as mixed slurry, then will be scattered Uniform pore creating material aqueous solution is slowly added to continue to stir in mixed slurry, is finally added dropwise to the slurry stirred evenly and divides at a high speed In scattered hot dimethicone, then conserving through baking oven, the synthetic product after maintenance is poured out from dimethicone, is filtered, is calcined, To obtain the final product.
- 2. the preparation method of porous geological polymer microballoon according to claim 1, it is characterised in that：It is described to swash with alkali The powder of hair activity is slag, slag, grain slag, flyash, silicon ash are divided, silicon powder, red mud, metakaolin, synthetic powder.
- 3. the preparation method of porous geological polymer microballoon according to claim 1, it is characterised in that：The aqueous slkali is Sodium silicate, potassium water glass, sodium hydroxide, potassium hydroxide, lithium hydroxide, strontium hydroxide, cesium hydroxide, carbonate, bicarbonate Salt, sulfate, disulfate, aluminate, the solution of aluminosilicate.
- 4. the preparation method of porous geological polymer microballoon according to claim 1, it is characterised in that：The pore creating material is Calcium carbonate, ammonium hydrogen carbonate, sodium acid carbonate, polyethylene glycol, polymethyl methacrylate, polyvinyl chloride, polyvinyl alcohol, alginic acid Sodium, polystyrene.
- 5. the preparation method of porous geological polymer microballoon according to claim 1, it is characterised in that comprise the following steps：(1) prepared by slurry：Powder with alkali-activated carbonatite activity and aqueous slkali are mixed evenly as mixed slurry, then will Finely dispersed pore creating material aqueous solution is slowly added to continue to stir in mixed slurry, is uniformly mixed, mixing speed 500-4000 Rev/min, stir 1-5 minutes, system is become homogeneous slurry；(2) balling-up：The homogeneous slurry of step (1) is added dropwise in the hot dimethicone of high speed dispersion；(3) cure：The dimethicone of step (2) and products therefrom are put into togerther in baking oven carry out it is curing；(4) filter：The dimethicone of step (3) and its products therefrom are subjected to vacuum filter, obtain geo-polymer microballoon；(5) calcine：The geo-polymer microballoon of step (4) is calcined in Muffle furnace, up to porous geological polymer microballoon.
- 6. the preparation method of porous geological polymer microballoon according to claim 1, it is characterised in that described in step (1) Powder with alkali-activated carbonatite activity is in terms of slag, and aqueous slkali is in terms of sodium silicate, and solvent is in terms of water, and pore creating material is with polymethyl Sour methyl esters meter, its mass ratio are slag: sodium silicate: water: polymethyl methacrylate=1: 0.1-1: 0.1-0.7: 0- 0.005。
- 7. the preparation method of porous geological polymer microballoon according to claim 1, it is characterised in that：The temperature of hot dimethicone is 40-150 degrees Celsius in step (2), and mixing speed is 200-2000 revs/min；In step (3) temperature of baking oven be 50-150 degrees Celsius, the curing time for 5 minutes -48 it is small when；The temperature of calcining is 200-900 degrees Celsius in step (5), when calcination time is 0.5-12 small.
- 8. porous geological polymer microballoon made from claim 1 is used as adsorbent.
- 9. porous geological polymer microballoon made from claim 1 is used as heavy metal or radioactive element adsorbent.
- 10. according to any adsorbent of claim 8 or 9, it is characterised in that：The porous geological polymer microballoon is put down Equal granularity is 5-500 microns, porosity 10-60%, specific surface area 20-120m2/g。
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