CN116459795A - Water treatment material for removing lead from wastewater and preparation method and application thereof - Google Patents
Water treatment material for removing lead from wastewater and preparation method and application thereof Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 239000002351 wastewater Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 75
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- 235000014787 Vitis vinifera Nutrition 0.000 claims abstract description 37
- 240000006365 Vitis vinifera Species 0.000 claims abstract description 37
- 150000002500 ions Chemical class 0.000 claims abstract description 26
- 239000010881 fly ash Substances 0.000 claims abstract description 23
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 20
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- 229940005550 sodium alginate Drugs 0.000 claims abstract description 20
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- 238000004108 freeze drying Methods 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
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- 238000000926 separation method Methods 0.000 claims abstract description 6
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- 238000001179 sorption measurement Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
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- 239000003463 adsorbent Substances 0.000 description 7
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Classifications
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- 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
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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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
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—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 physical properties
- B01J20/28009—Magnetic properties
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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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention belongs to the technical field of water treatment materials, and discloses a water treatment material for removing lead from wastewater, and a preparation method and application thereof, wherein the preparation method comprises the following steps: drying grape vine and bagasse, crushing, and uniformly mixing to obtain mixed powder; placing the mixed powder into a Fe-containing material 3+ Stirring the solution, and carrying out solid-liquid separation to obtain a precursor material; carbonizing a precursor material in a nitrogen atmosphere, grinding into powder, adding fly ash and alkali metal hydroxide, uniformly mixing, and performing activation treatment to obtain porous modified biochar; sodium alginate solution is used as embedding agent，CaCl 2 And (3) taking the solution as a cross-linking agent, carrying out gel embedding treatment on the porous modified biochar, and freeze-drying to obtain the water treatment material for removing lead from wastewater. The preparation method is simple to operate, and the prepared water treatment material can effectively adsorb lead ions, has excellent renewable and reusable performance, and is favorable for popularization and large-scale use.
Description
Technical Field
The invention relates to the technical field of water treatment materials, in particular to a water treatment material for removing lead from wastewater, and a preparation method and application thereof.
Background
At present, heavy metal pollution in China is more severe, especially lead ion pollution is caused, and crops absorb excessive lead ions to influence the growth and the yield of the crops; and lead ions are not biodegradable, so that the lead ions accumulate in animals and plants, thereby causing various diseases, and the durability and toxicity of the lead ions become one of main pollutants of water resources. Therefore, the problem of lead ion pollution in water environment is solved.
In the prior art, the most common methods for removing lead ions in wastewater are an electrolytic method, an ion exchange method, a membrane separation method and an adsorption method. The adsorption method has the advantages of simple operation, wide application range, no secondary pollution, high reaction speed, economy, good selectivity and easy design and operation, and is widely used. The adsorbent commonly used in the prior art comprises activated carbon, fly ash, magnetic graphene, chitosan and the like, but when the adsorbent is used for removing lead ions in water, the actual effective specific surface area is not high, so that the lead ion removing effect is poor, the adsorption treatment time is long, and the adsorbent is not beneficial to popularization and large-scale use. In order to improve the adsorbent material with a high specific surface area, those skilled in the art consider that a Metal Organic Framework (MOFs) is used as an adsorbent to remove lead ions in wastewater, but the Metal Organic Framework (MOFs) is poor in stability and selectivity, and cannot remove lead ions in wastewater efficiently.
Therefore, the invention provides a water treatment material for removing lead from wastewater, and a preparation method and application thereof.
Disclosure of Invention
In order to solve the technical problems, the invention provides a water treatment material for removing lead from wastewater, and a preparation method and application thereof.
The invention relates to a water treatment material for removing lead from wastewater, and a preparation method and application thereof, which are realized by the following technical scheme:
the first object of the present invention is to provide a method for preparing a water treatment material for lead removal from wastewater, comprising the steps of:
step 1, respectively drying grape vine and bagasse, and then crushing to obtain grape vine powder and bagasse powder; uniformly mixing the grape vine powder and bagasse powder to obtain mixed powder;
step 2, placing the mixed powder into a powder containing Fe 3+ Stirring the solution, and carrying out solid-liquid separation to obtain a precursor material;
step 3, carbonizing the precursor material in a nitrogen atmosphere to obtain modified biochar;
step 4, grinding the modified biochar into powder, adding fly ash and alkali metal hydroxide, uniformly mixing, and performing activation treatment to obtain porous modified biochar;
step 5, taking sodium alginate solution as embedding medium, caCl 2 And (3) taking the solution as a cross-linking agent, carrying out gel embedding treatment on the porous modified biochar, and freeze-drying to obtain the water treatment material for removing lead from wastewater.
Further, the mixed powder and the Fe-containing powder 2+ The dosage ratio of the solution is 1 g:15-25 mL;
and the Fe-containing 3+ Fe in solution 3+ The concentration of (C) is 0.8-1.2 mol/L.
Further, the mass ratio of the grape vine powder to the bagasse powder is 0.5-1.5:1.
Further, the mass ratio of the fly ash, the alkali metal hydroxide and the modified biochar is 1-3:0.2-0.5:1.
Further, the temperature of the stirring treatment is 65-75 ℃, and the stirring time is 20-60 min.
Further, the mass concentration of the sodium alginate solution is 2-4%; and the dosage ratio of the sodium alginate solution to the modified biochar is 10 mL:1-3 g.
Further, the CaCl 2 The mass concentration of the solution is 2-4%.
Further, the carbonization treatment process comprises the following steps:
firstly, heating to 300-400 ℃ at a heating rate of 5-10 ℃/min, preserving heat for 1-2 h, then heating to 500-600 ℃ at a heating rate of 10-15 ℃/min, preserving heat for 1-2 h, and then cooling to room temperature.
Further, the gel embedding treatment is performed by the following steps:
s1, uniformly dispersing the porous modified biochar in the sodium alginate solution to obtain a solution A;
s2, injecting the solution A into CaCl at the temperature of 3-5 DEG C 2 Obtaining gel microspheres in the solution;
s3, placing the gel microsphere for 0.5-1.5 h at room temperature, washing, and then adding CaCl 2 Immersing the surface of the water treatment material in the solution, then crosslinking for 18-24 hours at the temperature of 3-5 ℃, taking out the microspheres, washing and drying to obtain the water treatment material for removing lead from the wastewater.
A second object of the present invention is to provide a water treatment material prepared by the above preparation method.
A third object of the present invention is to provide an application of the above water treatment material in removing lead ions from wastewater.
Compared with the prior art, the invention has the following beneficial effects:
the invention takes grape vine powder and bagasse powder as carbon sources, and is prepared by immersing the grape vine powder and bagasse powder in Fe-containing solution 3+ In the solution, the grape vine powder and the bagasse powder are rich in plant fibers and pore structures, so that Fe can be conveniently loaded 3+ Further obtain Fe-loaded 3+ A carbon source, i.e., a precursor material. Then carbonizing the precursor material, wherein during carbonization, grape vine powder and bagasse powder are converted into biochar, and Fe is loaded on the biochar 3+ Conversion of ions to Fe 3 O 4 (and possibly Fe) 2 O 3 ) Obtaining the iron-modified biochar, wherein Fe 3 O 4 The magnetic property helps to separate the water treatment material from the aqueous phase well, so that it can be recovered quickly. And then, further modifying the modified biochar by taking the fly ash and the alkali metal hydroxide as a second modifier, wherein the fly ash contains a large number of porous glass bodies, is in a porous honeycomb structure, has a large specific surface area, and has a large number of active groups such as Si-O-Si bonds, al-O-Al bonds and the like on the surface, and has high adsorption activity. Moreover, the alkali metal hydroxide not only can further activate the modified biochar, but alsoCan assist the fly ash to generate a large number of new micro-pores under the high temperature condition, increase the specific surface area and the porosity, provide more sites for combining lead ions, effectively adsorb the lead ions, and further be beneficial to the adsorption performance. In addition, the gel material is coated on the surface of the biochar, so that the adsorption capacity of the material can be further improved, and the renewable and reutilization performance of the material is improved.
The preparation method is simple to operate, and the prepared water treatment material can effectively adsorb lead ions, has excellent renewable and reusable performance, and is favorable for popularization and large-scale use.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below.
The invention provides a water treatment material for removing lead from wastewater, which comprises the following preparation method:
step 1, respectively drying grape vine and bagasse, and then crushing to obtain grape vine powder and bagasse powder; uniformly mixing the grape vine powder and bagasse powder to obtain mixed powder;
the invention uses grape vine and bagasse as carbon source, which can not only relieve the pressure and pollution problem caused by the accumulation of agricultural wastes, but also realize the reutilization of resources and reduce the production cost. The grape vine powder and the bagasse powder are rich in plant fibers and pore structures, so that Fe is conveniently loaded 3+ Modification treatment is performed so as to introduce Fe 3 O 4 The isomagnetic molecules are favorable for separating the water treatment material from the water phase, so that the water treatment material can be recovered rapidly, and the problem that biochar powder is difficult to recover in the prior art is solved. And the mass ratio of the grape vine powder to the bagasse powder is preferably 0.5-1.5:1.
Wherein the temperature of the drying is 55-75 ℃ and the time is 4-8 h. And for convenience of Fe 3+ Loading, preferably crushing both grape vine and bagasse to 80 mesh sieve.
Step 2, mixing the componentsPlacing the powder in a Fe-containing device 3+ Stirring the solution, and carrying out solid-liquid separation to obtain a precursor material;
in the present invention, in order to make Fe 3+ Fully loaded on plant fiber and pore structure in grape vine powder and bagasse powder, preferably, the mixed powder and the Fe-containing powder 3+ The dosage ratio of the solution is 1 g:15-25 mL; and the Fe-containing 3+ Fe in solution 3+ The concentration of (C) is 0.8-1.2 mol/L. And the preferable stirring treatment temperature is 65-75 ℃, the stirring speed is 200-400 r/min, and the stirring time is 20-60 min.
Step 3, carbonizing the precursor material in a nitrogen atmosphere to obtain modified biochar;
in the invention, firstly, the precursor material is carbonized, so that the grape vine powder and bagasse powder are converted into biochar in the carbonization process of the precursor material, and Fe is loaded on the biochar 3+ Conversion of ions to Fe 3 O 4 (and possibly Fe) 2 O 3 ) Obtaining the iron-modified biochar, wherein Fe 3 O 4 The magnetic property helps to separate the water treatment material from the aqueous phase well, so that it can be recovered quickly. And the preferred carbonization treatment process is as follows: firstly, heating to 300-400 ℃ at a heating rate of 5-10 ℃/min, preserving heat for 1-2 h, then heating to 500-600 ℃ at a heating rate of 10-15 ℃/min, preserving heat for 1-2 h, and then cooling to room temperature.
Step 4, grinding the modified biochar into powder, adding fly ash and alkali metal hydroxide, uniformly mixing, and performing activation treatment to obtain porous modified biochar;
in order to enable the modified biochar to be fully contacted with the fly ash and the alkali metal hydroxide, the modified biochar needs to be ground into powder and ground before being mixed with the fly ash and the alkali metal hydroxide, so that the condition that excessive blocks are formed in the carbonization treatment and cannot be fully contacted with the fly ash and the alkali metal hydroxide is avoided, and the modified biochar is preferably ground to pass through a 100-mesh sieve.
The modified biochar is further modified by taking the fly ash and the alkali metal hydroxide as the second modifier, wherein the fly ash contains a large number of porous glass bodies, is in a porous honeycomb structure, has a large specific surface area, and has a large number of active groups such as Si-O-Si bonds, al-O-Al bonds and the like on the surface, and has high adsorption activity. In addition, the alkali metal hydroxide not only can further activate the modified biochar, but also can assist the fly ash to generate a large number of new micro-pores under the high temperature condition, increase the specific surface area and the porosity, provide more sites for combining lead ions, and effectively adsorb the lead ions, thereby being beneficial to the adsorption performance.
Step 5, taking sodium alginate solution as embedding medium, caCl 2 The solution is a cross-linking agent, gel embedding treatment is carried out on the porous modified biochar, and the water treatment material for removing lead from the wastewater is obtained after freeze drying;
the gel material is coated on the surface of the biochar, so that the adsorption capacity of the material can be further improved, and the renewable and reutilization performance of the material is improved. The gel embedding treatment is carried out by the following steps: s1, uniformly dispersing the porous modified biochar in the sodium alginate solution to obtain a solution A; s2, injecting the solution A into CaCl at the temperature of 3-5 DEG C 2 Obtaining gel microspheres in the solution; s3, placing the gel microsphere for 0.5-1.5 h at room temperature, washing, and then adding CaCl 2 Immersing the surface of the water treatment material in the solution, then crosslinking the water treatment material for 18-24 hours at the temperature of 3-5 ℃, taking out the microspheres, washing and freeze-drying the microspheres to obtain the water treatment material for removing lead from the wastewater.
The freeze-drying process according to the present invention is as follows: the freezing temperature is-45 to-55 ℃ and the time is 12 to 60 hours.
Then, the preparation method is simple to operate, and the prepared water treatment material can effectively adsorb lead ions, has excellent renewable and reusable performance, and is favorable for popularization and large-scale use.
Example 1
The embodiment provides a water treatment material for removing lead from wastewater, which is prepared by the following steps:
step 1, respectively drying grape vine and bagasse, and then crushing to obtain grape vine powder and bagasse powder; uniformly mixing the grape vine powder and bagasse powder to obtain mixed powder;
wherein the temperature of the drying is 60 ℃ and the time is 6 hours; and the particle sizes of the grape vine powder and the bagasse powder are all sieved by a 80-mesh sieve.
In this embodiment, the mass ratio of the grape vine powder to the bagasse powder is 1:1.
Step 2, placing the mixed powder into ferric trichloride solution with the concentration of 1.1mol/L, stirring for 40min at the stirring rate of 300r/min at the temperature of 70 ℃, and filtering to obtain a precursor material;
in this example, the ratio of the mixed powder to the ferric trichloride solution was 1 g/20 mL.
Step 3, carbonizing the precursor material in a nitrogen atmosphere, heating to 350 ℃ at a heating rate of 7 ℃/min for 1.5 hours, heating to 550 ℃ at a heating rate of 12 ℃/min for 1.5 hours, and cooling to room temperature to obtain modified biochar;
step 4, grinding the modified biochar into powder, sieving with a 100-mesh sieve to obtain biochar powder, adding fly ash and sodium hydroxide, uniformly mixing, and performing activation treatment to obtain porous modified biochar;
in this embodiment, the mass ratio of the fly ash, sodium hydroxide and the biochar is 2:0.3:1.
Step 5, taking sodium alginate solution as embedding medium, caCl 2 The solution is a cross-linking agent, the porous modified biochar is subjected to gel embedding treatment, and after drying, the water treatment material for removing lead from the wastewater is obtained;
in this embodiment, the gel embedding treatment is performed by the following steps:
s1, uniformly dispersing the porous modified biochar in a sodium alginate solution with the mass concentration of 3% to obtain a solution A; wherein the dosage ratio of the sodium alginate solution to the porous modified biochar is 10 mL/2 g;
s2, injecting the solution A to CaCl with the mass concentration of 4% at the temperature of 4 DEG C 2 Obtaining gel microspheres in the solution;
s3, placing the gel microsphere at room temperature for 1h, washing, and then adding CaCl with the mass concentration of 3 percent 2 Immersing the surface of the water treatment material in the solution, then crosslinking the water treatment material for removing lead from the wastewater at the temperature of 4 ℃ for 20 hours, taking out the microspheres, washing the microspheres, and drying the microspheres at the temperature of 60 ℃ for 3 hours to obtain the water treatment material for removing lead from the wastewater.
Example 2
The embodiment provides a water treatment material for removing lead from wastewater, which is prepared by the following steps:
step 1, respectively drying grape vine and bagasse, and then crushing to obtain grape vine powder and bagasse powder; uniformly mixing the grape vine powder and bagasse powder to obtain mixed powder;
wherein the temperature of the drying is 55 ℃ and the time is 4 hours; and the particle sizes of the grape vine powder and the bagasse powder are both 80-mesh sieves.
In this example, the mass ratio of the grape vine powder to the bagasse powder is 0.5:1.
Step 2, placing the mixed powder into a ferric trichloride solution with the concentration of 0.8mol/L, stirring for 20min at the stirring rate of 200r/min at the temperature of 65 ℃, and filtering to obtain a precursor material;
in this example, the ratio of the amount of the mixed powder to the amount of the ferric trichloride solution was 1 g/15 mL.
Step 3, carbonizing the precursor material in a nitrogen atmosphere, heating to 300 ℃ at a heating rate of 5 ℃/min for 1-2 h, heating to 500 ℃ at a heating rate of 10 ℃/min for 1h, and cooling to room temperature to obtain modified biochar;
step 4, grinding the modified biochar into powder, sieving with a 100-mesh sieve to obtain modified biochar powder, adding fly ash and sodium hydroxide, uniformly mixing, and performing activation treatment to obtain porous modified biochar;
in the embodiment, the mass ratio of the fly ash, the sodium hydroxide and the modified biochar is 1:0.2:1.
Step 5, taking sodium alginate solution as embedding medium, caCl 2 The solution is a cross-linking agent, the porous modified biochar is subjected to gel embedding treatment, and after drying, the water treatment material for removing lead from the wastewater is obtained;
in this embodiment, the gel embedding treatment is performed by the following steps:
s1, uniformly dispersing the porous modified biochar in a sodium alginate solution with the mass concentration of 2% to obtain a solution A; wherein the dosage ratio of the sodium alginate solution to the porous modified biochar is 10mL to 1g;
s2, injecting the solution A to CaCl with the mass concentration of 2% at the temperature of 3 DEG C 2 Obtaining gel microspheres in the solution;
s3, placing the gel microsphere at room temperature for 0.5h, washing, and then adding CaCl with the mass concentration of 2 percent 2 Immersing the surface of the water treatment material in the solution, then crosslinking the water treatment material for removing lead from the wastewater at the temperature of 3 ℃ for 18 hours, taking out the microspheres, washing the microspheres, and drying the microspheres at the temperature of 55 ℃ for 2 hours to obtain the water treatment material for removing lead from the wastewater.
Example 3
The embodiment provides a water treatment material for removing lead from wastewater, which is prepared by the following steps:
step 1, respectively drying grape vine and bagasse, and then crushing to obtain grape vine powder and bagasse powder; uniformly mixing the grape vine powder and bagasse powder to obtain mixed powder;
wherein the temperature of the drying is 65 ℃ and the time is 8 hours; and the particle sizes of the grape vine powder and the bagasse powder are both 80-mesh sieves.
In this example, the mass ratio of the grape vine powder to the bagasse powder is 1.5:1.
Step 2, placing the mixed powder into ferric trichloride solution with the concentration of 1.2mol/L, stirring at the stirring rate of 400r/min for 60min at the temperature of 75 ℃, and filtering to obtain a precursor material;
in this example, the ratio of the amount of the mixed powder to the amount of ferric trichloride solution was 1 g/25 mL.
Step 3, carbonizing the precursor material in a nitrogen atmosphere, heating to 400 ℃ at a heating rate of 10 ℃/min for 2 hours, heating to 600 ℃ at a heating rate of 15 ℃/min for 2 hours, and cooling to room temperature to obtain biochar;
step 3, grinding the biochar into powder, sieving with a 100-mesh sieve to obtain biochar powder, adding fly ash and potassium hydroxide, uniformly mixing, and performing activation treatment to obtain modified biochar;
in this embodiment, the mass ratio of fly ash, potassium hydroxide and biochar is 3:0.5:1.
Step 4, taking sodium alginate solution as an embedding agent and CaCl 2 The solution is a cross-linking agent, gel embedding treatment is carried out on the modified biochar, and the water treatment material for removing lead from the wastewater is obtained after drying;
in this embodiment, the gel embedding treatment is performed by the following steps:
s1, uniformly dispersing the modified biochar in a sodium alginate solution with the mass concentration of 4% to obtain a solution A; wherein the dosage ratio of the sodium alginate solution to the modified biochar is 10 mL/3 g;
s2, injecting the solution A to CaCl with the mass concentration of 4% at the temperature of 5 DEG C 2 Obtaining gel microspheres in the solution;
s3, placing the gel microsphere at room temperature for 1.5h, washing, and then adding CaCl with the mass concentration of 4 percent 2 Immersing the surface of the water treatment material in the solution, then crosslinking the water treatment material for removing lead from the wastewater at the temperature of 5 ℃ for 24 hours, taking out the microspheres, washing the microspheres, and drying the microspheres at the temperature of 65 ℃ for 4 hours to obtain the water treatment material for removing lead from the wastewater.
Comparative example 1
This comparative example provides a water treatment material for lead removal from wastewater and differs from example 1 only in that:
the comparative example was modified without addition of fly ash and sodium hydroxide.
Comparative example 2
This comparative example provides a water treatment material for lead removal from wastewater and differs from example 1 only in that:
the comparative example was not subjected to gel embedding treatment.
Comparative example 3
This example provides a water treatment material for lead removal from wastewater and differs from example 1 only in that:
the comparative example does not use Fe 3+ And (3) carrying out modification treatment on the solution, namely directly carbonizing the mixed powder.
Comparative example 4
This example provides a water treatment material for lead removal from wastewater and differs from example 1 only in that:
this comparative example uses only bagasse powder as the carbon source.
Test section
The invention uses certain industrial waste liquid as waste liquid to be treated, and the concentration of lead ions is 8.58mg/L through detection.
And the water treatment materials prepared in the embodiment 1 and the comparative examples 1-3 are used as adsorbents, 20g of the water treatment materials are respectively placed in 1L of waste liquid to be treated, the pH is regulated to 6, the water treatment materials are stirred at the room temperature for 60min at the rotating speed of 150r/min, the concentration of lead ions in the water treatment materials is detected after solid-liquid separation, the lead ion removal rate is calculated, and the lead ion removal rate is recorded as shown in the table 1.
In the invention, the lead ion concentration detection and removal rate calculation are carried out: the lead ion concentration in the waste liquid is measured according to inductively coupled plasma emission spectrometry (HJ 776-2015) for measuring 32 elements in water. The lead ion removal rate was calculated according to the following formula:wherein R is Pb For lead ion removal rate, c Pb0 C for initial concentration of lead ions (mg/L) in the pre-treatment waste liquid Pbt The concentration (mg/L) of lead ions in the treated waste liquid is shown.
TABLE 1 lead ion removal Rate
The water treatment material prepared in the embodiment 1 is taken as an adsorbent, placed in the 1L waste liquid to be treated, pH value is regulated to 6, stirred and adsorbed at the room temperature for 60min at the rotating speed of 150r/min, and after adsorption is finished, ethanol is used for washing 3 times to carry out desorption, then the water treatment material is placed in a drying oven at the temperature of 60 ℃ to be dried for 4 hours, and then is used for adsorbing lead ions again, and desorption regeneration is repeated for 5 times to carry out 5 times of adsorption-desorption experiment tests, and the test shows that the removal rate of the lead ions is 94.1%, 93.8%, 91.4%, 89.1% and 85.6% respectively, which shows that the adsorption capacity of the water treatment material prepared in the embodiment 1 on the lead ions is reduced, but is still not lower than 90% of the first adsorption effect, and the water treatment material prepared in the embodiment has good desorption regeneration performance.
It should be apparent that the embodiments described above are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Claims (10)
1. The preparation method of the water treatment material for removing lead from wastewater is characterized by comprising the following steps of:
step 1, respectively drying grape vine and bagasse, and then crushing to obtain grape vine powder and bagasse powder; uniformly mixing the grape vine powder and bagasse powder to obtain mixed powder;
step 2, placing the mixed powder into a powder containing Fe 3+ Stirring the solution, and carrying out solid-liquid separation to obtain a precursor material;
step 3, carbonizing the precursor material in a nitrogen atmosphere to obtain modified biochar;
step 4, grinding the modified biochar into powder, adding fly ash and alkali metal hydroxide, uniformly mixing, and performing activation treatment to obtain porous modified biochar;
step 5, taking sodium alginate solution as embedding medium, caCl 2 And (3) taking the solution as a cross-linking agent, carrying out gel embedding treatment on the porous modified biochar, and freeze-drying to obtain the water treatment material for removing lead from wastewater.
2. The method according to claim 1, wherein the mixed powder and the Fe-containing powder are mixed together 3+ The dosage ratio of the solution is 1 g:15-25 mL;
and the Fe-containing 3+ Fe in solution 3+ The concentration of (C) is 0.8-1.2 mol/L.
3. The method of claim 1, wherein the mass ratio of grape vine powder to bagasse powder is 0.5-1.5:1.
4. The method according to claim 1, wherein the mass ratio of the fly ash, the alkali metal hydroxide and the modified biochar is 1-3:0.2-0.5:1.
5. The method according to claim 1, wherein the stirring treatment is carried out at a temperature of 65 to 75℃for 20 to 60 minutes.
6. The preparation method of claim 1, wherein the mass concentration of the sodium alginate solution is 2-4%; the dosage ratio of the sodium alginate solution to the porous modified biochar is 10 mL:1-3 g;
the CaCl 2 The mass concentration of the solution is 2-4%.
7. The method of claim 1, wherein the carbonization process comprises:
firstly, heating to 300-400 ℃ at a heating rate of 5-10 ℃/min, preserving heat for 1-2 h, then heating to 500-600 ℃ at a heating rate of 10-15 ℃/min, preserving heat for 1-2 h, and then cooling to room temperature.
8. The preparation method according to claim 1, wherein the gel embedding treatment is performed by:
s1, uniformly dispersing the porous modified biochar in the sodium alginate solution to obtain a solution A;
s2, injecting the solution A into CaCl at the temperature of 3-5 DEG C 2 Obtaining gel microspheres in the solution;
s3, placing the gel microsphere for 0.5-1.5 h at room temperature, washing, and then adding CaCl 2 Immersing the surface of the water treatment material in the solution, then crosslinking the water treatment material for 18-24 hours at the temperature of 3-5 ℃, taking out the microspheres, washing and freeze-drying the microspheres to obtain the water treatment material for removing lead from the wastewater.
9. A water treatment material prepared by the method of any one of claims 1 to 8.
10. Use of a water treatment material according to claim 9 for removing lead ions from wastewater.
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| CN117486438B (en) * | 2024-01-03 | 2024-04-02 | 北京哈泰克工程技术有限公司 | Treatment method of desulfurization wastewater of power plant |
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