CN117244519A - Composite porous Si@Al adsorbent prepared by utilizing electric flocculation precipitation waste, method and application thereof - Google Patents
Composite porous Si@Al adsorbent prepared by utilizing electric flocculation precipitation waste, method and application thereof Download PDFInfo
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- CN117244519A CN117244519A CN202311531702.8A CN202311531702A CN117244519A CN 117244519 A CN117244519 A CN 117244519A CN 202311531702 A CN202311531702 A CN 202311531702A CN 117244519 A CN117244519 A CN 117244519A
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- 239000002699 waste material Substances 0.000 title claims abstract description 40
- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 37
- 229910021426 porous silicon Inorganic materials 0.000 title claims abstract description 35
- 238000005189 flocculation Methods 0.000 title claims abstract description 26
- 230000016615 flocculation Effects 0.000 title claims abstract description 26
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- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 28
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- GSDSWSVVBLHKDQ-UHFFFAOYSA-N 9-fluoro-3-methyl-10-(4-methylpiperazin-1-yl)-7-oxo-2,3-dihydro-7H-[1,4]oxazino[2,3,4-ij]quinoline-6-carboxylic acid Chemical compound FC1=CC(C(C(C(O)=O)=C2)=O)=C3N2C(C)COC3=C1N1CCN(C)CC1 GSDSWSVVBLHKDQ-UHFFFAOYSA-N 0.000 description 1
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N Nitrogen dioxide Chemical class O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- JCCZVLHHCNQSNM-UHFFFAOYSA-N [Na][Si] Chemical compound [Na][Si] JCCZVLHHCNQSNM-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0248—Compounds of B, Al, Ga, In, Tl
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—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 surface properties or porosity
-
- 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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- 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
- C02F2101/30—Organic compounds
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
-
- 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
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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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
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention belongs to the field of materials, and discloses a method for preparing a composite porous Si@Al adsorbent by utilizing electric flocculation precipitation waste, and an application thereof, wherein the method comprises the following steps: the raw materials adopt the precipitation waste generated in the electric flocculation water treatment process; adding chlorella liquid into the precipitated waste; illuminating and vibrating; filtering, grinding and sieving; mixing with sodium silicate; calcining 2 h to obtain the composite porous Si@Al adsorbent. The preparation method is simple and easy to implement, and the adsorbent can adsorb various pollutants such as organic matters, antibiotics, heavy metals and the like at the same time, so that the problems of high raw material cost and difficult adsorption of the existing adsorbent are successfully solved; the adsorbent has the advantages of strong adsorption performance, short adsorption time, wide applicable pH range and high repeated use rate, and realizes waste recycling. The test result can provide reference for the preparation of the low-cost adsorption material, and can also provide a new thought for recycling the electric flocculation precipitation waste.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a composite porous Si@Al adsorbent prepared by utilizing electric flocculation precipitation waste, a method and application thereof.
Background
Antibiotics and heavy metals are widely applied to agriculture, industry, medical industry and the like, so that the pollution of the antibiotics and the heavy metals in the environment, especially the water environment, is caused, and the fluidity and the solubility characteristics of the antibiotics and the heavy metals are further aggravated. Up to now, water pollution has become a considerable environmental problem, seriously affecting the economic and social development of China and the health of people.
The method for simultaneously removing the antibiotics and the heavy metals mainly comprises an adsorption method and a membrane separation method, and compared with the adsorption method, the adsorption method is a method for efficiently and simultaneously removing the antibiotics and the heavy metals due to low cost, simple operation and high removal rate. The adsorption materials commonly used in adsorption methods generally include carbon-based materials, metal-organic frameworks, mineral materials, mesoporous materials, and the like. Among them, metal-related materials perform well, but are generally expensive; the performance of minerals and carbon-based raw materials is limited, the removal effect of certain pollutants is poor, performance improvement is usually required to improve the efficiency, most of the current technologies pay attention to modified materials, however, various chemical agents are usually required to be added in the modification process for soaking or pickling, and even strong acid, strong alkali, heavy metal solution and the like are used for modification, so that the operation can greatly increase the cost, and a great deal of toxic and harmful waste liquid is worried about.
Therefore, the invention prepares the composite porous Si@Al adsorbent by using precipitated waste generated after the electric flocculation water treatment, doping a small amount of sodium silicate powder and simply calcining at 200 ℃. The preparation process has the advantages of low cost of raw materials, no use of toxic and harmful chemical substances, no generation of waste liquid, simple steps, great time saving and economic cost, environmental friendliness, excellent performance and wide adaptability, and can simultaneously remove organic matters, antibiotics and heavy metals in sewage.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a method for preparing a composite porous Si@Al adsorbent by utilizing electric flocculation precipitation waste, and application thereof.
The technical scheme adopted for solving the technical problems is as follows:
a method for preparing a composite porous Si@Al adsorbent by utilizing electroflocculation precipitation waste comprises the following steps:
(1) The raw materials adopt the precipitation waste generated in the electric flocculation water treatment process;
(2) Adding chlorella concentrate into the precipitate waste, wherein the final mass concentration of the chlorella concentrate is 0.5%, and placing the mixture in an illumination incubator at 26 ℃ under 3500lx illumination 2 h; simultaneously, vibrating the mixed solution at 120 rpm;
wherein the chlorella concentrate is a solid substance formed by filtering chlorella liquid, and polyethylene glycol is added for soaking for 10 min, and the solid substance is: the mass of the polyethylene glycol is 1:1;
meanwhile, the algae cells are uniformly distributed on the colloid network structure, ca and Mg plasmas in the water body are easily combined to the surface on the surfaces of the microalgae cells, and 'hole points' are formed in the subsequent calcination.
(3) Filtering the mixed solution after shaking in the step (2), naturally air-drying the precipitate or drying the precipitate at 60 ℃, grinding the precipitate, and sieving the precipitate with a 60-mesh sieve to obtain uniform precipitate powder;
(4) Mixing the precipitate powder obtained in the step (3) with sodium silicate in a powder-powder mixing manner to obtain a mixture;
(5) Calcining the mixture in the step (4) at the temperature of 200 ℃ for 2 h to obtain the composite porous Si@Al adsorbent.
Further, the precipitated waste in the step (1) is generated by industrial hydropower flocculation to remove silicon, and the initial concentration of the silicon is 10-60 mg/L; the anode plate is an aluminum (Al) electrode and the cathode plate is a stainless steel electrode when the silicon is removed by electric flocculation;
the electric flocculation uses a direct current power supply, and the current density is 3.2 mA/cm 2 The distance between the polar plates is 0.5 and cm, the water inflow rate is 0.25 and L/min, and the hydraulic retention time is 10 and s.
Moreover, unlike chemical substances having a crystal structure, the precipitate is Al which slowly separates out under the action of a weak electric field 3+ The polymer has good uniformity and dispersibility, huge specific surface area and more active sites with thin and interweaved reticular colloid formed by chemical bonds, such as O, H, si.
Further, the mixing of the precipitate powder in step (4) with sodium silicate is performed in air, and the addition of liquid affects the performance of the adsorbent.
The sodium silicate forms a 'cauliflower-shaped' composite hole with surrounding sediment during calcination, so that the specific surface area and the porosity of the adsorbent are further improved.
Further, the precipitate powder in step (4): the mass ratio of the sodium silicate is 1:1 to 6:1.
the composite porous Si@Al adsorbent prepared by the method is prepared.
The application method of the composite porous Si@Al adsorbent comprises the following steps:
and (3) weighing the composite porous Si@Al adsorbent, and directly putting the composite porous Si@Al adsorbent into a water body for adsorption operation.
The regeneration method of the composite porous Si@Al adsorbent comprises the following steps:
the regeneration method of the composite porous Si@Al adsorbent after use is solvent regeneration or calcination regeneration.
The use of a composite porous si@al adsorbent as described above for the simultaneous adsorption of a plurality of contaminants.
Further, the plurality of contaminants include organics, antibiotics, heavy metals.
The invention has the advantages and positive effects that:
1. the adsorbent of the invention does not need to be soaked or reacted by toxic and harmful chemical substances or washed by a large amount of water in the preparation process, so that toxic and harmful waste liquid is not generated. The chemical reagent used in the preparation process is only a small amount of sodium silicate, and the chemical reagent is directly mixed with powder, so that no waste liquid or secondary pollutant is generated, and the environmental ecological effect is better.
2. The preparation method of the invention has simple and easy preparation process and low cost. The adsorbent uses industrial waste as raw materials, and expensive heavy metals, chemicals and other expensive chemical substances are not used in the preparation process, so that the material cost is low. The calcining condition in the preparation process is that the calcining condition is 200 ℃ and the calcining condition is 2 h, which is lower than the temperature (450-800 ℃) and the processing time (soaking and calcining are approximately 50 h) which are commonly used in the prior art, so the energy consumption is low and the time cost is low.
3. The adsorbent of the present invention is excellent in effect. The adsorbent has good adsorption performance on various pollutants with different properties (organic matters, antibiotics, heavy metals and the like); the adsorbent has short adsorption time (10-30 min) which is lower than a plurality of hours in the prior art; the adsorbent has high adsorption efficiency, wide applicable pH range (2.5-10) and high repeated use rate.
4. The adsorbent dissolves only a small amount of Al in the use process 3+ And silicate, does not dissolve out heavy metalsAnd toxic and harmful substances or ions, so that the adsorbent is safer and more effective in use.
5. The preparation method of the adsorbent disclosed by the invention uses waste to treat waste, does not generate secondary pollution, can provide a treatment route of changing waste into valuable, is green and efficient for water treatment, and accords with the green development concept.
Drawings
FIG. 1 is a graph showing the adsorption performance of adsorbents produced by different mass ratios of precipitated waste powder to sodium silicate in example 1 of the present invention;
FIG. 2 is a graph showing the adsorption performance of adsorbents produced at different muffle temperatures in example 1 of the present invention;
FIG. 3 is a graph showing the adsorption performance of the adsorbents prepared under different mixing conditions in example 1 of the present invention;
FIG. 4 is an XRD pattern of the adsorbent of example 1 of the present invention; wherein A is XRD pattern of Si@Al adsorbent, and B is XRD pattern of electric flocculation precipitation waste raw material;
FIG. 5 is a Scanning Electron Microscope (SEM) image of the microstructure of the adsorbent of example 1 of the present invention;
FIG. 6 is a graph showing the adsorption effect of Si@Al adsorbents of different mass concentrations on methylene blue in example 2 of the present invention;
FIG. 7 is a graph showing the adsorption capacity of the adsorbent of example 2 of the present invention for methylene blue at various initial concentrations over time;
FIG. 8 is a graph showing the effect of Si@Al adsorbent in example 2 of the present invention on methylene blue adsorption at different pH values;
FIG. 9 is a graph showing the recycling of Si@Al adsorbent to methylene blue in example 2 of the present invention;
FIG. 10 is a graph showing the adsorption capacity of Si@Al adsorbent for tetracycline over time in example 3 of the present invention;
FIG. 11 is a graph showing the effect of Si@Al adsorbent in example 3 of the present invention on adsorption of tetracycline at different temperatures;
FIG. 12 shows the weight of the Si@Al adsorbent to heavy metal Cd in example 3 of the invention 2+ A plot of adsorption capacity over time;
FIG. 13 shows Si in example 3 of the present inventionAt different temperatures for Cd by the @ Al adsorbent 2+ Adsorption effect graph of (2).
Detailed Description
The invention will now be further illustrated by reference to the following examples, which are intended to be illustrative, not limiting, and are not intended to limit the scope of the invention.
The various experimental operations involved in the specific embodiments are conventional in the art, and are not specifically noted herein, and may be implemented by those skilled in the art with reference to various general specifications, technical literature or related specifications, manuals, etc. before the filing date of the present invention.
A method for preparing a composite porous Si@Al adsorbent by utilizing electroflocculation precipitation waste comprises the following steps:
(1) The raw materials adopt the precipitation waste generated in the electric flocculation water treatment process;
(2) Adding chlorella concentrate into the precipitate waste, wherein the final mass concentration of the chlorella concentrate is 0.5%, and placing the mixture in an illumination incubator at 26 ℃ under 3500lx illumination 2 h; simultaneously, vibrating the mixed solution at 120 rpm;
wherein the chlorella concentrate is a solid substance formed by filtering chlorella liquid, and polyethylene glycol is added for soaking for 10 min, and the solid substance is: the mass of the polyethylene glycol is 1:1;
meanwhile, the algae cells are uniformly distributed on the colloid network structure, ca and Mg plasmas in the water body are easily combined to the surface on the surfaces of the microalgae cells, and 'hole points' are formed in the subsequent calcination.
(3) Filtering the mixed solution after shaking in the step (2), naturally air-drying the precipitate or drying the precipitate at 60 ℃, grinding the precipitate, and sieving the precipitate with a 60-mesh sieve to obtain uniform precipitate powder;
(4) Mixing the precipitate powder obtained in the step (3) with sodium silicate in a powder-powder mixing manner to obtain a mixture;
(5) Calcining the mixture in the step (4) at the temperature of 200 ℃ for 2 h to obtain the composite porous Si@Al adsorbent.
Preferably, the precipitated waste in the step (1) is generated by industrial hydropower flocculation to remove silicon, and the initial concentration of the silicon is 10-60 mg/L; the anode plate is an aluminum (Al) electrode and the cathode plate is a stainless steel electrode when the silicon is removed by electric flocculation;
the electric flocculation uses a direct current power supply, and the current density is 3.2 mA/cm 2 The distance between the polar plates is 0.5 and cm, the water inflow rate is 0.25 and L/min, and the hydraulic retention time is 10 and s.
Moreover, unlike chemical substances having a crystal structure, the precipitate is Al which slowly separates out under the action of a weak electric field 3+ The polymer has good uniformity and dispersibility, huge specific surface area and more active sites with thin and interweaved reticular colloid formed by chemical bonds, such as O, H, si.
Preferably, the mixing of the precipitate powder in step (4) with sodium silicate is performed in air, and the addition of liquid affects the performance of the adsorbent.
The sodium silicate forms a 'cauliflower-shaped' composite hole with surrounding sediment during calcination, so that the specific surface area and the porosity of the adsorbent are further improved.
Preferably, the precipitate powder in step (4): the mass ratio of the sodium silicate is 1:1 to 6:1.
the composite porous Si@Al adsorbent prepared by the method is prepared.
The application method of the composite porous Si@Al adsorbent comprises the following steps:
and (3) weighing the composite porous Si@Al adsorbent, and directly putting the composite porous Si@Al adsorbent into a water body for adsorption operation.
The regeneration method of the composite porous Si@Al adsorbent comprises the following steps:
the regeneration method of the composite porous Si@Al adsorbent after use is solvent regeneration or calcination regeneration.
The use of a composite porous si@al adsorbent as described above for the simultaneous adsorption of a plurality of contaminants.
Preferably, the plurality of contaminants includes organics, antibiotics, heavy metals.
Specifically, the related preparation and detection are as follows:
example 1: preparation and characterization of Si@Al adsorbent under different conditions
Weighing naturally air-dried electric flocculation silicon removal sediment, wherein the sediment waste is generated by removing silicon through industrial hydropower flocculation, and the initial concentration of the silicon is 10-60 mg/L; the anode plate is an aluminum (Al) electrode and the cathode plate is a stainless steel electrode when the silicon is removed by electric flocculation; the electric flocculation uses a direct current power supply, and the current density is 3.2 mA/cm 2 The distance between the polar plates is 0.5 and cm, the water inflow rate is 0.25 and L/min, and the hydraulic retention time is 10 and s. Adding chlorella concentrate with final mass concentration of 0.5% into the precipitate waste, and placing in an illumination incubator at 26 ℃ under 3500lx illumination of 2 h; simultaneously, vibrating the mixed solution at 120 rpm; the chlorella concentrate is a solid substance formed by filtering chlorella liquid, and polyethylene glycol is added for soaking for 10 min, wherein the solid substance is: the mass of the polyethylene glycol is 1:1.
Filtering the mixed solution after oscillation, naturally air-drying the precipitate or drying the precipitate at 60 ℃, grinding the precipitate, and sieving the precipitate with a 60-mesh sieve to obtain uniform precipitate powder; the mass ratio of the dried precipitated waste powder to the sodium silicate is respectively 0.5:1, 1:1, 4:1, 6:1, 10:1 and 20:1, and the mixing conditions are set as follows: mixing the dry powders, adding water, ethanol, and Tween 80. Placing the materials in a crucible uniformly, setting the muffle furnace temperature to be 200, 300, 400, 500 and 700 ℃, calcining the materials to be 2.0 and h, and naturally cooling the materials. Adsorbents under different conditions were prepared.
As can be seen from fig. 1 to 3, the si@al adsorbents prepared under different conditions have a certain adsorption performance, but the adsorption performance of the adsorbents prepared under different conditions is different, and as a whole, when the precipitate powder: the mass ratio of the sodium silicate is 4:1, the temperature is 200 ℃, and the adsorption performance of the adsorbent prepared by mixing the powder is best. The microscopic morphology of the si@al adsorbent was characterized by Scanning Electron Microscopy (SEM), the results are shown in fig. 5. The figure shows that the adsorbent has uniform flower shape, uniform particle size, distinct layers and loose and porous performance after calcination at 200 ℃, which indicates that the obvious porous medium adsorbent appearance is formed. FIG. 4 is an XRD pattern showing that neither the electroflocculation desilication precipitation waste nor the Si@Al adsorbent formed after calcination has distinct characteristic diffraction peaks, which indicates that the material exhibits an amorphous structure inside.
Example 2: preparation of Si@Al adsorbent, and adsorption effect and recycling of Si@Al adsorbent on methylene blue
The Si@Al adsorbent was prepared as in example 1, wherein the mass ratio of precipitate to sodium silicate was 4: and 1, uniformly mixing the materials in an air medium in a powder-powder mixing mode, calcining 2.0 and h at the muffle temperature of 200 ℃, and naturally cooling. The adsorbents with different mass concentrations (2, 4, 6, 8 g/L and 10 g/L) are added into 10 mL methylene blue-containing solution, and the mixture is vibrated for 30 min at 100 rpm in a vibrating box at 25 ℃ to determine the concentration of the methylene blue by spectrophotometry.
As can be seen from FIGS. 6 and 7, the methylene blue removal rate was as high as 90.77% at 30 min when the amount of the adsorbent was 4 g/L, the removal rate could be increased by 94.27% by continuing to increase the amount of the adsorbent, and the removal rate could be increased by 99.2% if the adsorption time was continued to increase to 60 min. As shown in fig. 8, the removal rate of the adsorbent at different pH values can be seen to have a good removal effect in the pH value range of 4-10, and the change of the pH value hardly affects the removal rate (the change is not significant p > 0.05). As shown in fig. 9, the removal rate was reduced by about 6% after 5 times of use, and the recycling rate was high, in view of the influence of the recycling times.
Example 3: preparation of Si@Al adsorbent, adsorption effect of Si@Al adsorbent on tetracycline and heavy metal and recycling
The Si@Al adsorbent was prepared as in example 1, wherein the mass ratio of precipitate to sodium silicate was 4: and 1, uniformly mixing the materials in an air medium in a powder-powder mixing mode, calcining 2.0 and h at the muffle temperature of 200 ℃, and naturally cooling. Adding 10 mL of adsorbent containing tetracycline and Cd to obtain a mixture of different mass concentrations 2+ In a shaking box at 25 ℃, shaking for 30 min at 100 rpm, and determining the concentration of the tetracycline by utilizing a high performance liquid chromatography-mass spectrometry/mass spectrometry combined technology.
As can be seen from FIGS. 10 and 11, when the amount of the adsorbent was increased from 0.0 mg/5 mL to 0.01 mg/5 mL, the removal rate of tetracycline increased to 80.93%, and when the reaction time was 10 min, the removal rate of tetracycline reached 97.85%, which indicates that Si@Al adsorbed tetracycline very rapidly and adsorption equilibrium was reached in 10 min. The effect of different temperatures on tetracycline removal was not apparent. As is clear from fig. 12 and 13, the removal rate after 5 times of use is reduced by about 8% and the recycling rate is high, from the influence of the recycling times. When the amount of the adsorbent was increased from 0.0 mg/10 mL to 0.04 mg/10 mL, the removal rate of Cd increased to 96.44%; the influence of different pH values on the tetracycline removal rate is not obvious; from the influence of the recycling times, the removal rate is reduced by about 3% after the recycling is performed for 5 times, and the recycling rate is high.
Example 4: comparison of sodium silicate and calcium hydroxide added in preparation of Si@Al adsorbent
The preparation method of the Si@Al adsorbent is as in example 1, wherein the precipitate and sodium silicate or calcium hydroxide are mixed in an air medium in a powder-powder mixing mode, and the mixing mass ratio is 4:1, calcining 2.0. 2.0 h at the muffle temperature of 200 ℃ and naturally cooling. Adding adsorbent with mass concentration of 6.0. 6.0 g/L into 10 mL solutions containing different methylene blue concentrations (100, 300, 500 mg/L), shaking at 100 rpm for 30 min in a shaking box at 25deg.C, and spectrophotometrically measuring the methylene blue concentration.
As can be seen from Table 1, the adsorption performance of the adsorbent prepared by doping sodium silicate is significantly better than that of the adsorbent prepared by doping calcium hydroxide, and particularly, at a higher initial concentration, the adsorption capacity of the adsorbent prepared in the invention is higher, for example, when the initial methylene blue concentration is 500 mg/L, the adsorption capacity of the adsorbent prepared by mixing with sodium silicate and calcining after 30 min is 81.93 mg/g, and the adsorption capacity of the adsorbent prepared by doping calcium hydroxide and calcining is only 54.64 mg/g. From the viewpoint of the equilibrium time of adsorption, the time for the adsorbent prepared by doping sodium silicate to reach equilibrium is shorter, the adsorbent prepared by mixing with sodium silicate only needs 5-15 min to reach the equilibrium of adsorption, and the time for the adsorbent prepared by mixing with calcium hydroxide to reach the equilibrium of adsorption is about 15-30 min. In conclusion, the adsorbent prepared by mixing with sodium silicate has more excellent performance.
TABLE 1 adsorption Capacity of sodium silicate and calcium hydroxide doped adsorbents for methylene blue (mg/g)
Meanwhile, as can be seen from comparative examples 1 and 4, the steps of mixing sodium silicate with precipitate powder and sodium silicate in a powder-powder mixing manner in the preparation method of the invention have a synergistic effect, and the relative performance of the prepared composite porous Si@Al adsorbent can be synergistically improved.
Example 5: si@Al adsorbents of the present invention are compared to adsorbents of other technologies
The preparation method of the Si@Al adsorbent is as in example 1, wherein the precipitate is mixed with sodium silicate or calcium hydroxide in an air medium, and the mixing mass ratio is 4:1, calcining 2.0. 2.0 h at the muffle temperature of 200 ℃ and naturally cooling. The performance of the prepared adsorbent is compared with the adsorbent effect in the prior art in many ways.
Table 2 compares in detail the type of adsorbent, the preparation conditions, the experimental conditions and the removal effect on the target in the different studies. From the source of raw materials, the invention uses industrial solid waste, which not only has zero cost, but also can lighten the solid waste treatment pressure of enterprises and generate environmental effect. From the viewpoint of the preparation method, most of the existing adsorbents have long preparation flow, and various other compounds can be used, so that the cost of the medicament is greatly increased; the calcination temperature is usually high (450-800 ℃), even nitrogen environment or a large amount of water is used for flushing, so that resources are wasted and time cost is increased. In addition, the amount of adsorbent used in this study was 1 g.L -1 ~3 g•L -1 Substantially identical to or even lower than the amount of adsorbent used in the other studies (0.5 g.L -1 ~5 g•L -1 ). From the aspect of reaction time, the adsorbent realizes the adsorption process of antibiotics and heavy metal ions within 30 min, and partial researches can be completed in a few hours, so that the adsorbent has the advantage of time and cost. From the viewpoint of the removal efficiency, the Si@Al adsorbent in the invention also has good effectAs a result, the adsorption efficiency was significantly higher than in some studies. In summary, the adsorbent in the invention has remarkable advantages in various aspects and can be widely used for adsorbing and removing pollutants with different properties.
Table 2 si@al adsorbents vs. other adsorbents in literature
Adsorbents A kind of electronic device with a display unit | Preparation method | Pollution of target Article (B) | Initial concentration (mg·L -1 ) | For adsorbents Quantity (g.L) -1 ) | Removal rate of (%) | Preparation method Environmental effects of (2) Should be |
Penicillin bacterium Slag biochar | Penicillin bacterium Slag and water-free Potassium carbonate to Mass ratio 1:1 Proportion of addition of Deionized water is used for preparing the water, impregnation activation 2 h, centrifuging and mixing Drying; at nitrogen In the air atmosphere, the air is filled in the air cavity, at 10 DEG C min -1 Heating up To 600 ℃,2 h, performing H; with 3 mol·L -1 Salt Soaking in acid to remove Ion water washing To neutral and and (5) drying. | Tetracycline | 200 | 1 | 99.91% (120min) | Calcination temperature High; generating a large Measuring waste liquid |
Sludge organisms Quality charcoal; sludge treatment Activated carbon | 24 g dry dirt Mud addition 136 g ultrapure water Mixing, 260 Heating at 10 DEG C h, performing H; after centrifugation Precipitation leaching Soaking in dilute salt In acid (5%) 10 h, ultra-pure Repeated water cleaning Washing the mixture to be neutral, drying to obtain Sludge organisms And (5) quality charcoal. Sludge treatment Biomass charcoal With ZnCl 2 Mixing Combining, impregnating 10 h, drying; under nitrogen atmosphere Under the atmosphere respectively 500 to Calcining at 700 DEG C 90 min; by using Ultrapure water reverse Number of rewashing Secondary, drying is carried out, thus obtaining the sewage Mud activated carbon. | Tetracycline, head Sodium ceftriaxone, Erythromycin and erythromycin Ofloxacin | 50 | 1.0~1.5 | 10.92%(60 min); 99.93% (30 min) | Calcination temperature High; generating a large Waste liquid (containing Zn) |
Typha root Charcoal | Typha and KOH Mass ratio of (2) 3:1 blend Combining and ultrasound treatment The treatment is carried out for 20 min; in nitrogen atmosphere In the middle of the circumference, 450 Calcination at 1 DEG C h, at 800 again Calcination at 1 DEG C h, performing H; sample the sample Grinding and using 0.5 mol· L -1 HCl and HCl Deionized water Alternate washing Several times until The washing liquid is Neutral; at 60 Drying oven at DEG C Middle drying 48 h。 | TC and Cr (VI) | TC (50) Cr(VI) (5) | 1.0 | 99.50% (90 min) and 95.77%(90 min) | calcination temperature High; generating a large Measuring waste liquid |
Nano Fe 3 O 4 Acid-loading modification Sexual charcoal | 12.108 g FeCl 3 · 6H 2 O and 4.452 g FeCl 2 · 4H 2 o is dissolved and then dissolved, 200-220 r·min -1 Stirring Stirring for 20 min; add 5.000 g initial coconut shell Biomass charcoal Stirring 2 h; add 60 mL Concentrated ammonia water in Water at 50 DEG C Bath and stirring Reaction 3 h; by deionization Washing with water to Eluent electric appliance Conductivity is reduced to 100 μS· cm -1 In the following the procedure is described, absolute ethyl alcohol The washing is carried out for 3 times, drying at 60 DEG C Drying 12 and h; adding 100mL of Nitro Acid (65% -65) 68%),90℃ Water bath 3 h; by deionization Washing with water to Eluent electric appliance Conductivity is reduced to 100 μS· cm- 1 The following is given. | Pb 2+ 、Cd 2+ | 300 | 5 | 52% (6 h)、42% (6 h) | Generating a large amount of Organic and inorganic Waste liquid |
Nano zero-valent Iron (Fe) | 100mL none Ethanol/water Separating in solution Are added separately to FeCl 2 · 4H 2 O, let in High purity nitrogen 30 min, by turns Gradually add 50 mL(0. 5 mol·L -1 ) NaBH 4 Dissolving solution Liquid, firstly use without Oxygen water flushing 3 Pass through, reuse without Washing with water and ethanol 3 Pass through, finally will Prepared material The temperature of the material is 60 DEG C Air drying 12 h。 | Pb 2+ | 200~600 | 0.5 | 84.3%~ 100% (20 ~60 min) | Generating harmful effects Waste liquid |
Si@Al adsorption Agent | Precipitation and disposal Object and pellet Algae concentrate Mixing and air drying The preparation of the powder is carried out, powder and silicon Sodium acid in 4:1 The mass ratio of the components is as follows, calcination at 200 DEG C 2 h。 | TC、Cr、Pb | TC (2~ 20)、Cd (7.5~ 90)、Pb (40~540) | 1.0~3.0 | 98.02%~ 99.99% (30 min) | Calcination temperature Low; does not produce Waste liquid |
Although embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that: various substitutions, changes and modifications are possible without departing from the spirit and scope of the invention and the appended claims, and therefore the scope of the invention is not limited to the disclosure of the embodiments.
Claims (9)
1. A method for preparing a composite porous Si@Al adsorbent by utilizing electric flocculation precipitation waste is characterized by comprising the following steps of: the method comprises the following steps:
(1) The raw materials adopt the precipitation waste generated in the electric flocculation water treatment process;
(2) Adding chlorella concentrate into the precipitate waste, wherein the adding mass concentration of the chlorella concentrate is 0.5%, and placing the mixture in an illumination incubator at 26 ℃ under 3500lx illumination 2 h; simultaneously, vibrating the mixed solution at 120 rpm;
wherein the chlorella concentrate is a solid substance formed by filtering chlorella liquid, and polyethylene glycol is added for soaking for 10 min, and the solid substance is: the mass of the polyethylene glycol is 1:1;
(3) Filtering the mixed solution after shaking in the step (2), naturally air-drying the precipitate or drying the precipitate at 60 ℃, grinding the precipitate, and sieving the precipitate with a 60-mesh sieve to obtain uniform precipitate powder;
(4) Mixing the precipitate powder obtained in the step (3) with sodium silicate in a powder-powder mixing manner to obtain a mixture;
(5) Calcining the mixture in the step (4) at the temperature of 200 ℃ for 2 h to obtain the composite porous Si@Al adsorbent.
2. The method according to claim 1, characterized in that: the precipitated waste in the step (1) is generated by industrial hydropower flocculation to remove silicon, and the initial concentration of the silicon is 10-60 mg/L; the anode plate is an aluminum electrode and the cathode plate is a stainless steel electrode when the silicon is removed by electric flocculation;
the electric flocculation uses a direct current power supply, and the current density is 3.2 mA/cm 2 The distance between the polar plates is 0.5 and cm, the water inflow rate is 0.25 and L/min, and the hydraulic retention time is 10 and s.
3. The method according to claim 1, characterized in that: the precipitate powder in step (4) is mixed with sodium silicate in air.
4. The method according to claim 1, characterized in that: precipitate powder in step (4): the mass ratio of the sodium silicate is 1:1 to 6:1.
5. a composite porous si@al adsorbent prepared by the method of any one of claims 1 to 4.
6. The method for using the composite porous Si@Al adsorbent according to claim 5, wherein the method comprises the following steps of: the method comprises the following steps:
and (3) weighing the composite porous Si@Al adsorbent, and directly putting the composite porous Si@Al adsorbent into a water body for adsorption operation.
7. The method for regenerating a composite porous si@al adsorbent according to claim 6, wherein: the method comprises the following steps:
the regeneration method of the composite porous Si@Al adsorbent after use is solvent regeneration or calcination regeneration.
8. Use of a composite porous si@al adsorbent according to claim 5 for the simultaneous adsorption of a plurality of contaminants.
9. The use according to claim 8, characterized in that: the plurality of pollutants comprise organic matters, antibiotics and heavy metals.
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JP2002059001A (en) * | 2000-08-11 | 2002-02-26 | Okutama Kogyo Co Ltd | Anion adsorbent |
CN102294227A (en) * | 2011-06-30 | 2011-12-28 | 国家海洋局天津海水淡化与综合利用研究所 | Preparation method and application method of chlorella seawater purifying biological adsorbent |
CN106946434A (en) * | 2017-03-24 | 2017-07-14 | 合肥供水集团有限公司 | A kind of resource utilization method of water treatment plant's contained manganess aluminium iron sludge |
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JPH02164406A (en) * | 1988-12-19 | 1990-06-25 | Merusu Giken:Kk | Pretreatment of granular filter medium |
JP2002059001A (en) * | 2000-08-11 | 2002-02-26 | Okutama Kogyo Co Ltd | Anion adsorbent |
CN102294227A (en) * | 2011-06-30 | 2011-12-28 | 国家海洋局天津海水淡化与综合利用研究所 | Preparation method and application method of chlorella seawater purifying biological adsorbent |
CN106946434A (en) * | 2017-03-24 | 2017-07-14 | 合肥供水集团有限公司 | A kind of resource utilization method of water treatment plant's contained manganess aluminium iron sludge |
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