CN110041016B - Geopolymer adsorbing material and preparation method thereof - Google Patents
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- CN110041016B CN110041016B CN201910300343.2A CN201910300343A CN110041016B CN 110041016 B CN110041016 B CN 110041016B CN 201910300343 A CN201910300343 A CN 201910300343A CN 110041016 B CN110041016 B CN 110041016B
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Abstract
The invention provides a geopolymer adsorbing material and a preparation method thereof, wherein the geopolymer adsorbing material comprises the following raw materials in parts by weight: the preparation method comprises the steps of uniformly mixing the raw materials to obtain slurry, injecting the slurry into a mold, and alternately maintaining at 80 ℃ and room temperature to obtain the geopolymer adsorbing material. The geopolymer adsorbing material with low cost and high adsorption performance is prepared by using the fly ash, the metakaolin and the like as raw materials, so that on one hand, a new material is provided for removing heavy metal ions in sewage, on the other hand, the resource utilization of industrial waste is realized, and the application prospect is good.
Description
Technical Field
The invention relates to the field of adsorption materials, in particular to a geopolymer adsorption material and a preparation method thereof.
Background
The industrial wastewater containing heavy metals is discharged into the environment without being treated, so that the soil and water are polluted, and the growth and the survival of animals and plants are adversely affected. Heavy metals can ultimately harm human health after entering the body through the food chain. Industries such as electroplating, battery manufacturing, printed circuit boards, and metal surface coating treatment are important sources for generating sewage containing heavy metals.
At present, methods for purifying heavy metals in water include membrane separation technology, ion exchange technology, biological treatment technology, adsorption method, chemical precipitation and the like. The adsorption method is widely applied to sewage treatment due to the characteristics of convenience, high efficiency, low cost and the like. The traditional adsorbing materials comprise natural adsorbing materials (such as zeolite, kaolin, diatomite, montmorillonite, wood fiber and the like), artificial adsorbing materials (such as activated carbon, carbon nanotubes, nanofiber membranes and the like) and biological adsorbing materials (bacteria, fungi, algae and the like), but the adsorbing materials still have the problems of poor adsorption performance, high application cost and the like, so that the adsorbing materials cannot be popularized and applied in a large range.
The geopolymer is an inorganic polymer formed by condensation of aluminosilicate mineral powder and alkali solution at the temperature of below 100 ℃, and has a three-dimensional polymeric structure and abundant pores. Geopolymers exhibit superior properties in terms of durability, freeze-thaw resistance, abrasion resistance, fire resistance, etc., and thus are widely used in the construction field and filling materials. In addition, the geopolymer also has the characteristics of high strength, acid and alkali resistance, heat resistance and the like, and is widely applied to the field of curing and stabilizing treatment of toxic wastes. The invention aims to provide a geopolymer adsorption material with good adsorption performance and low cost.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a geopolymer adsorbing material and a preparation method thereof.
The invention aims at providing a geopolymer adsorbing material which comprises the following raw materials in parts by weight: 15-35 parts of fly ash, 65-85 parts of metakaolin, 40-120 parts of water glass, 2-30 parts of sodium hydroxide and 30-90 parts of deionized water.
According to the technical scheme, the fly ash, the metakaolin, the sodium hydroxide, the water glass and the deionized water are used as raw materials, the Si/Al ratio of the geopolymer is adjusted by adjusting the proportion of the fly ash to the metakaolin, and the Si/Na ratio of the geopolymer is adjusted by adjusting the proportion of the sodium hydroxide to the water glass, so that the prepared geopolymer adsorption material has good pressure resistance and large specific surface area, and particularly has excellent heavy metal adsorption performance.
Preferably, the geopolymer adsorbing material comprises the following raw materials in parts by weight: 30-35 parts of fly ash, 65-75 parts of metakaolin, 60-70 parts of water glass, 10-20 parts of sodium hydroxide and 30-50 parts of deionized water.
Preferably, the metakaolin is prepared by calcining raw kaolin ore powder at 800-1000 ℃ for 2-3 h.
Further preferably, the metakaolin is prepared by calcining raw kaolin ore powder at 900 ℃ for 3 hours.
Preferably, the mesh number of the fly ash and the metakaolin is not less than 100 meshes.
Preferably, the modulus of the water glass is 1-4, and more preferably 3.1-3.4.
The second purpose of the invention is to provide a preparation method of the geopolymer adsorbing material, wherein the raw materials are uniformly mixed to obtain slurry, the slurry is injected into a mold, and alternate curing is carried out at 80 ℃ and room temperature (15-35 ℃) to obtain the geopolymer adsorbing material.
Preferably, the preparation method specifically comprises the following steps:
(1) uniformly mixing the fly ash and metakaolin to obtain aluminosilicate powder;
(2) mixing water glass and sodium hydroxide, carrying out ultrasonic treatment for 10-30 min, and standing for 12-48 h to obtain an alkali activator;
(3) mixing and stirring the aluminosilicate powder, the alkali activator and deionized water to obtain a geopolymer homogenate;
(4) and injecting the geopolymer homogenate into a mold, sealing, performing alternate maintenance at 80 ℃ and room temperature to obtain a geopolymer block, crushing, and sieving with a 30-mesh sieve to obtain the geopolymer adsorbing material.
Preferably, the specific conditions for curing in step (4) are as follows: curing for 12 hours under the sealing condition of 80 ℃, curing for 12 hours under the sealing condition of room temperature, curing for 12 hours under the sealing condition of 80 ℃, curing for 7 days under the sealing condition of room temperature, and curing for 7 days under the ventilation condition of room temperature.
Preferably, the geopolymer block in step (4) is crushed, sieved, and then washed and air-dried by deionized water under the following washing conditions: the solid-liquid mass ratio is 1:10, and the washing procedure is that the washing is performed by oscillating at room temperature for 8 hours, water bath washing at 90 ℃ for 5 hours, washing for 2 times, oscillating at room temperature for 8 hours and washing for 3 times.
As a preferred embodiment of the present invention, the preparation method of the geopolymer adsorption material comprises the following steps:
(1) firstly, preparing raw materials in parts by weight: 30-35 parts of fly ash, 65-75 parts of metakaolin, 60-70 parts of water glass, 10-20 parts of sodium hydroxide and 30-50 parts of deionized water;
(2) uniformly mixing the fly ash and metakaolin to obtain aluminosilicate powder;
(3) mixing water glass and sodium hydroxide, carrying out ultrasonic treatment for 10-30 min, and standing for 12-48 h to obtain an alkali activator;
(4) mixing and stirring the aluminosilicate powder, the alkali activator and deionized water to obtain a geopolymer homogenate;
(5) and (3) after the geopolymer homogenate is injected into a mould for sealing, maintaining: curing for 12 hours under the sealing condition of 80 ℃, curing for 12 hours under the sealing condition of room temperature, curing for 12 hours under the sealing condition of 80 ℃, curing for 7 days under the sealing condition of room temperature, and curing for 7 days under the ventilation condition of room temperature to obtain geopolymer blocks, and crushing and sieving by a 30-mesh sieve to obtain the geopolymer adsorbing material.
The third purpose of the invention is to provide the application of the geopolymer adsorbing material or the preparation method thereof in the fields of heavy metal adsorption, heavy metal pollution treatment and heavy metal recovery.
According to the invention, the geopolymer adsorbing material with low cost and high adsorption performance is prepared by using the fly ash, the metakaolin and the like as raw materials and adjusting the proportion of the raw materials and the maintenance conditions, so that a new material is provided for removing heavy metal ions in sewage, the resource utilization of industrial waste is realized, and the application prospect is good. The geopolymer adsorbing material disclosed by the invention is used for adsorbing Pb in solution2+、Cd2+、Cu2+The saturated adsorption amounts of the components are 40.68-154.11 mg/g and 30.56-78.23 mg/g respectivelyAnd 11.64-36.61 mg/kg. The preparation process and equipment of the invention have simple conditions and low cost, and are suitable for large-scale production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 shows the adsorption of Pb in solution by a geopolymer adsorbent at different adsorption times in example 2 of the present invention2+A graph of change in the amount of adsorption of (c);
FIG. 2 shows the application of geopolymer adsorbing materials to Cd in solution under different adsorption time conditions in example 2 of the present invention2+A graph of change in the amount of adsorption of (c);
FIG. 3 shows the adsorption of Cu in solution by geopolymer adsorbent at different adsorption times in example 2 of the present invention2+A graph of change in the amount of adsorption of (c);
FIG. 4 shows the adsorption of geopolymer materials for Pb in solution at different initial concentrations in example 3 of the present invention2+A graph of change in adsorption amount and removal rate of (a);
FIG. 5 shows the Geopolymer adsorbent material on Cd in solution at different initial concentrations in example 3 of the present invention2+A graph of change in adsorption amount and removal rate of (a);
FIG. 6 shows the Geopolymer adsorbent material versus Cu in solution at different initial concentrations in example 3 of the present invention2+A graph showing the change in the adsorption amount and the removal rate.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1 preparation of geopolymer adsorbent Material
The embodiment provides a geopolymer adsorbing material which comprises the following raw materials in parts by weight: 33.3 parts of fly ash, 66.7 parts of metakaolin, 65.6 parts of water glass, 14.4 parts of sodium hydroxide and 40 parts of deionized water;
wherein, the metakaolin is prepared by calcining kaolin raw ore powder for 3 hours at 900 ℃, and the fly ash and the metakaolin are respectively sieved by a 100-mesh sieve; the water glass modulus was 3.3.
The preparation method of the geopolymer adsorbing material comprises the following steps:
(1) uniformly mixing the fly ash and metakaolin to obtain aluminosilicate powder;
(2) mixing water glass and sodium hydroxide, carrying out ultrasonic treatment for 20min, and standing at room temperature for 24h to obtain an alkali activator;
(3) mixing the aluminosilicate powder obtained in the step (1), the alkali activator obtained in the step (2) and deionized water, and stirring at a rotating speed of 540r/min for 30min to obtain a geopolymer homogenate;
(4) and (4) injecting the geopolymer homogenate obtained in the step (3) into a mould for sealing, and then maintaining: curing at the sealing condition of 80 ℃ for 12 hours, curing at the sealing condition of room temperature for 12 hours, curing at the sealing condition of 80 ℃ for 12 hours, curing at the sealing condition of room temperature for 7 days, and curing at the ventilating condition of room temperature for 7 days to obtain geopolymer blocks, and crushing and sieving with a 30-mesh sieve to obtain geopolymer particles;
(5) washing the geopolymer particles obtained in the step (4) with deionized water, wherein the solid-liquid mass ratio is 1:10, the washing procedure is that the geopolymer particles are washed by shaking at room temperature for 8 h-washing in a 90 ℃ water bath for 5h, washed for 2 times-washing by shaking at room temperature for 8h and washed for 3 times, and the geopolymer adsorbing material of the target product is obtained after air drying.
The room temperature in the preparation method is 15-35 ℃.
Example 2 adsorption of heavy metal ions in solution at various time conditions using the geopolymer adsorbent material of example 1
Using Pb (NO)3)2、Cd(NO3)2And Cu (NO)3)2Preparing heavy metal solutions with certain concentration by using reagents respectively, and using NaOH and HNO3The pH of the solution is adjusted. Weighing 0.1g of geopolymer adsorbing material, adding the geopolymer adsorbing material into 25ml of heavy metal solution, oscillating at 25 ℃, and adsorbing heavy metal under different time conditions. The adsorption solution was filtered through a microporous membrane having a pore size of 0.45 μm, and the concentration of heavy metal ions in the solution was measured by an atomic absorption method.
Wherein the initial concentration and initial pH of heavy metal ions in each solution are respectively as follows: pb2+300mg/L，pH＝3；Cd2+300mg/L，pH＝5；Cu2+200mg/L, pH 4. The adsorption time gradients were set as: 0.5, 10, 20, 40, 80, 120, 180, 240, 300, 400, 600 min.
Geopolymer adsorbing material for Pb in solution under different adsorption time conditions2+、Cd2+、Cu2+The change in the amount of adsorption of (c) is shown in FIGS. 1 to 3. As can be seen from the figure, the geopolymer adsorbent material is specific to Pb in solution2+、Cd2+、Cu2+The time for the adsorption to reach the equilibrium is 240min, 300min and 240min respectively, and the equilibrium adsorption capacity is 70.76, 57.14 and 14.64mg/g respectively. Based on the above results, the equilibrium time for the geopolymer adsorbent to adsorb heavy metals in the solution was set to 300 min.
Example 3 adsorption of heavy metals at different concentrations using the Geopolymer adsorbent material of example 1
Using Pb (NO)3)2、Cd(NO3)2、Cu(NO3)2Preparing heavy metal solutions with different concentration gradients by using NaOH and HNO respectively3The pH of the solution is adjusted. Pb2+The initial pH of (1) was set to 3, and the initial concentration gradient was set to 100, 200, 300, 500, 800, 1000 mg/L; cd [ Cd ]2+The initial pH of (1) was set to 5, and the initial concentration gradient was set to 50, 100, 200, 300, 500, 800 mg/L; cu2+Was set to 4, and the initial concentration gradient was set to 50, 100, 200, 300, 500 mg/L.
Weighing 0.1g of geopolymer adsorbing material, adding the geopolymer adsorbing material into 25ml of heavy metal solution, and oscillating for 300min at 25 ℃ to balance adsorption. The adsorption solution was filtered through a microporous membrane having a pore size of 0.45 μm, and the concentration of heavy metal ions in the solution was measured by an atomic absorption method.
Geopolymer adsorbing material for Pb in solution under different initial concentration conditions2+、Cd2+、Cu2+The changes in the adsorption amount and the removal rate of (c) are shown in fig. 4 to 6. As can be seen from the figure, the geopolymer adsorbent material is for Pb2+、Cd2+、Cu2+The maximum adsorption capacity of the adsorbent can reach 154.11, 78.23 and 36.61mg/g respectively. Pb in solution2+When the concentration of (A) is less than 500mg/L, the adsorbing material is used for adsorbing Pb2+The removal rate of (2) is above 91.57%; cd in solution2+When the concentration of the adsorbent is less than 300mg/L, the adsorbent is used for adsorbing Cd2+The removal rate of (A) is more than 98.22%; cu in solution2+When the concentration of (A) is less than 100mg/L, the adsorbent is aligned with Cu2+The removal rate of (2) is 95.17% or more.
Comparative example 1
The difference from the example 1 lies in the curing process: the geopolymer slurry was cured at room temperature for 14 days. The resulting product easily turned into a paste in water.
Comparative example 2
The difference from example 1 is that the aluminosilicate powder contained only fly ash.
Comparative example 3
The difference from example 1 is that the aluminosilicate powder contains only metakaolin.
Comparative example 4
The difference from the example 1 is that the aluminosilicate powder is metakaolin and zeolite, and the mass ratio is 3: 1; the curing method comprises sealing and curing at 50 deg.C for 24 hr, cooling at room temperature, soaking in tap water, and curing at room temperature for 28 days. The curing time required by the curing mode is far longer than that of the invention.
Comparative example 5
The geopolymer adsorbing material provided by the comparative example comprises the following raw materials in parts by weight: 62 parts of fly ash, 40 parts of metakaolin, 75 parts of water glass, 33 parts of sodium hydroxide and 40 parts of deionized water, and the preparation method is the same as that of example 1.
Geopolymer adsorbent of comparative examples 2-5 Pb was carried out as in example 32+、Cu2+、Cd2+The adsorption test (2) was conducted to examine the maximum adsorption amount of the heavy metal by each adsorbent, and the results are shown in Table 1.
TABLE 1 maximum adsorption of heavy metals by Geopolymer adsorbent materials
As can be seen from the above table, the geopolymer adsorbing material prepared by the invention has good Pb-tolerance2+、Cd2+And Cu2+The maximum adsorption amounts of the lead-free adsorbent and the lead-free adsorbent can reach 154.11, 78.23 and 36.61mg/g respectively, while the adsorption materials prepared by the comparative example have the effect of adsorbing Pb2+、Cd2+And Cu2+The maximum adsorption capacity ranges are 126.64-136.51 mg/g, 52.82-69.47 mg/g and 25.51-30.94 mg/g respectively, and the adsorption capacity is obviously inferior to that of the geopolymer adsorption material prepared by the invention.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (7)
1. The geopolymer adsorbing material is characterized by comprising the following raw materials in parts by weight: 30-35 parts of fly ash, 65-75 parts of metakaolin, 60-70 parts of water glass, 10-20 parts of sodium hydroxide and 30-50 parts of deionized water;
the metakaolin is prepared by calcining raw kaolin ore powder at 800-1000 ℃ for 2-3 h;
the preparation method of the geopolymer adsorbing material comprises the following steps: and uniformly mixing the raw materials to obtain slurry, injecting the slurry into a mold, and alternately maintaining at 80 ℃ and room temperature to obtain the geopolymer adsorbing material.
2. The geopolymer adsorbent material of claim 1, wherein said metakaolin is prepared from kaolin crude ore powder calcined at 900 ℃ for 3 hours.
3. The geopolymer adsorbent material of claim 1 or 2, wherein said fly ash and said metakaolin have a mesh size of no less than 100 mesh.
4. A preparation method of the geopolymer adsorbing material as claimed in any one of claims 1 to 3, characterized in that the raw materials are uniformly mixed to obtain slurry, the slurry is injected into a mold, and alternate curing is performed at 80 ℃ and room temperature to obtain the geopolymer adsorbing material.
5. The method for preparing a geopolymer adsorbent material according to claim 4, characterized in that it comprises the following steps:
(1) uniformly mixing the fly ash and metakaolin to obtain aluminosilicate powder;
(2) mixing water glass and sodium hydroxide, carrying out ultrasonic treatment for 10-30 min, and standing for 12-48 h to obtain an alkali activator;
(3) mixing and stirring the aluminosilicate powder, the alkali activator and deionized water to obtain a geopolymer homogenate;
(4) and injecting the geopolymer homogenate into a mold, sealing, performing alternate maintenance at 80 ℃ and room temperature to obtain a geopolymer block, crushing, and sieving with a 30-mesh sieve to obtain the geopolymer adsorbing material.
6. The method for preparing a geopolymer adsorbing material according to claim 5, wherein the specific conditions for curing in the step (4) are as follows: curing for 12 hours under the sealing condition of 80 ℃, curing for 12 hours under the sealing condition of room temperature, curing for 12 hours under the sealing condition of 80 ℃, curing for 7 days under the sealing condition of room temperature, and curing for 7 days under the ventilation condition of room temperature.
7. Use of the geopolymer adsorbing material according to any one of claims 1 to 3 or the preparation method according to any one of claims 4 to 6 in the fields of heavy metal adsorption, heavy metal pollution treatment and heavy metal recovery.
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| FR3106507B1 (en) * | 2020-01-28 | 2024-03-01 | Commissariat Energie Atomique | SOLID MATERIAL WITH MULTIPLE OPEN POROSITY COMPRISING A GEOPOLYMER AND SOLID PARTICLES AND PREPARATION METHOD THEREFOR |
| CN111250039B (en) * | 2020-03-13 | 2021-10-19 | 常熟理工学院 | Method for preparing hydroxyapatite functionalized geopolymer adsorbent by using tuff |
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| CN113426421B (en) * | 2021-06-30 | 2022-07-22 | 深圳信息职业技术学院 | Foamed geopolymer adsorption material and preparation method and application thereof |
| CN113387627A (en) * | 2021-07-26 | 2021-09-14 | 昆明理工大学 | Method for fixing lead by steel slag-metakaolin based polymer material |
| CN113620306B (en) * | 2021-08-24 | 2022-11-18 | 广西民族大学 | Flower-type zeolite molecular sieve, preparation method and application thereof |
| CN113831068B (en) * | 2021-09-29 | 2022-09-06 | 南京信息工程大学 | Preparation method and application of porous geopolymer material |
| CN113908805B (en) * | 2021-11-15 | 2022-12-20 | 东北大学 | Carbon nano tube reinforced inorganic adsorbent, preparation method and application thereof |
| CN115869580B (en) * | 2022-11-29 | 2024-03-01 | 贵州大学 | Mercury tailing curing agent and use method thereof |
| CN116078343A (en) * | 2022-12-07 | 2023-05-09 | 上海蓝科石化环保科技股份有限公司 | Adsorbent for removing heavy metals in waste gas and preparation method thereof |
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| CN105289469A (en) * | 2015-10-31 | 2016-02-03 | 中国地质大学（武汉） | Geopolymer based porous adsorption material and preparation method thereof |
| CN108298846A (en) * | 2018-04-16 | 2018-07-20 | 葛潇楠 | A kind of geopolymer gelled material and preparation method |
| CN109400016A (en) * | 2018-09-29 | 2019-03-01 | 盐城工学院 | Geo-polymer porous insulation material and preparation method thereof based on burning city domestic garbage bottom ash |
| CN109574558A (en) * | 2018-11-20 | 2019-04-05 | 东北大学秦皇岛分校 | One kind is based on iron tailings geo-polymer porous material and preparation method thereof |
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