CN113354046A - Carbon nitride modified nano Fe3O4Application of material as algae inhibitor and method - Google Patents
Carbon nitride modified nano Fe3O4Application of material as algae inhibitor and method Download PDFInfo
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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- 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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- 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
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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
- C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
- C02F1/488—Treatment of water, waste water, or sewage with magnetic or electric fields for separation of magnetic materials, e.g. magnetic flocculation
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Abstract
The invention discloses a carbon nitride modified nano Fe3O4The application and method of the material as algae inhibitor; the carbon nitride modified nano Fe3O4Passing the material through nano Fe3O4And carbon nitride as precursor, and calcining to obtain nano Fe3O4The mass ratio of the carbon nitride to the carbon nitride is 1: 5-2: 1. The invention uses the nano Fe modified by carbon nitride3O4The material is used for inhibiting algae. The material can rapidly remove algae cells in solution during algae inhibiting process, and form magnetic material with easy settlingA descending floc; under the condition of an external magnetic field, the flocculate can be quickly settled, so that the algae liquid is quickly clarified and transparent, and the recovery and the reutilization of materials and algae cell flocculate are facilitated. In addition, the carbon nitride modified nano Fe used in the invention3O4The reusability of the material is better. The method saves resources and time, and achieves the same or higher algae removal efficiency than the existing algae removal process.
Description
Technical Field
The invention relates to carbon nitride modified nano Fe3O4Of materialsA preparation method and application in the algae inhibiting process, belonging to the technical field of water pollution treatment.
Background
At present, the eutrophication phenomenon of water body caused by the discharge of a large amount of nitrogen and phosphorus elements is serious, blue algae bloom frequently appears all over the world, the bloom outbreak can consume dissolved oxygen in water and destroy the aquatic ecological balance, wherein the blue algae are the most common algae causing the bloom outbreak, and the blue algae can cause the color and the odor of the water body during the bloom outbreak and release a large amount of algal toxins into the water body along with the death of cells, thereby seriously harming aquatic organisms and the health of human beings. Therefore, it is imperative to find an economically sound method to effectively remove algae growth.
Nano Fe3O4As a magnetic nano material, the magnetic nano material is widely applied to the technical field of water pollution treatment due to good magnetism, and can effectively recover the material under the condition of an external magnetic field. However, nano Fe3O4In the technical field of water pollution treatment, the method is mainly used for synergistically enhancing the photocatalytic performance of other materials and the recovery performance of the materials, and a water treatment process utilizing the good magnetic flocculation performance of the materials is provided.
The graphite phase carbon nitride has high hardness, biocompatibility and chemical stability, and the material has small average pore size, concentrated pore channel structure and high porosity and is widely applied to the technical fields of adsorption and photocatalysis. In the aspect of controlling cyanobacterial bloom, carbon nitride is mostly used as a substrate of a photocatalytic material, and the good adsorbability of the carbon nitride is less utilized to inhibit algae synergistically. The carbon nitride is used as a modifier to prepare a material which is not photocatalytic and can rapidly remove algae in water through good adsorbability, and more attention and more intensive research are needed.
At present, metal oxide modified by carbon nitride is often used as a photocatalyst to be applied to the field of controlling cyanobacterial bloom outbreak. However, various photocatalysts have the following problems in practical application, including unobvious algae inhibition effect, too long treatment time, difficulty in recovering materials, generation of toxic by-products and the like. At present, the carbon nitride is not used for modifying the nano Fe3O4Related algae inhibiting material and method for removing soluble organic matter in water bodyAnd (5) related reports of pollutants. Under the condition of an external magnetic field, whether the material can synergistically enhance the algae inhibition effect is unknown.
Disclosure of Invention
Aiming at the technical problems, the invention provides carbon nitride modified nano Fe3O4Material, nano Fe modified by carbon nitride3O4Algae inhibition is carried out through the synergistic effect of the two components, and meanwhile, soluble organic pollutants in the water body are removed in the process, so that harmful algae in the water body are effectively removed, and the materials are recycled.
In a first aspect, the invention provides carbon nitride modified nano Fe3O4The material is applied as an algae inhibitor.
Preferably, the carbon nitride modified nano Fe3O4In the material, nano Fe3O4The mass ratio of the carbon nitride to the carbon nitride is 1: 5-2: 1.
Preferably, the carbon nitride modified nano Fe3O4In the material, nano Fe3O4And the mass ratio of carbon nitride is 1: 3.
In a second aspect, the algae inhibiting method comprises the following specific processes: modifying the carbon nitride with nano Fe3O4The material was added to the treated algal solution and stirring was applied.
Preferably, the carbon nitride modified nano Fe3O4The amount of the material used is 1.0-5.0 g/L relative to the algae liquid to be treated.
Preferably, a magnetic field is applied to the algae liquid to be treated. The source of the magnetic field is positioned at the bottom of the treated algae liquid, so that the carbon nitride modified nano Fe3O4The algae adsorbed by the material can settle quickly. After the algae inhibiting treatment is finished, flocs settled under the action of a magnetic field are collected. The obtained flocculate is cleaned and recycled to obtain reusable carbon nitride modified nano Fe3O4A material.
In a third aspect, the carbon nitride modified nano Fe is provided3O4The preparation method of the material comprises the following specific steps:
step one, mixing carbon nitride and nano Fe3O4And (4) mixing. The mixing process comprises mixing, drying, grinding, and sieving to obtain solid mixture.
Step two, calcining the solid mixture obtained in the step one, and cooling to room temperature to obtain the carbon nitride modified nano Fe3O4A material.
Preferably, the nano Fe3O4And the mass ratio of the carbon nitride to the carbon nitride is 2: 1-1: 5.
Preferably, the mixing method in the first step is as follows: mixing nano Fe3O4Placing the mixture and carbon nitride in a preparation container, adding absolute ethyl alcohol, uniformly stirring, then carrying out ultrasonic treatment and drying treatment, and carrying out grinding and 60-mesh sieve screening to obtain a solid mixture in a dark brown powder shape.
Preferably, the carbon nitride in the first step is obtained by calcining dicyandiamide as a precursor; the calcination conditions were: heating to 500 deg.C at a heating rate of 10 deg.C/min in a box-type atmosphere furnace, calcining at 500 deg.C for 2 hr, heating to 520 deg.C at a heating rate of 5 deg.C/min, calcining at 520 deg.C for 2 hr, and naturally cooling to room temperature. The calcination conditions in the second step are as follows: heating a muffle furnace to 450 ℃, putting the muffle furnace into a crucible containing the solid mixture obtained in the step one, calcining the mixture at 450 ℃ for 2 hours, and naturally cooling the calcined mixture to room temperature to obtain brown solid powdery carbon nitride modified nano Fe3O4A material.
The invention has the beneficial effects that:
1. the invention uses the nano Fe modified by carbon nitride3O4The material is used for inhibiting algae. The material can quickly remove algae cells in the solution in the process of inhibiting algae, and flocculate which has magnetism and is easy to settle is formed, so that the recovery and the reutilization of the material and the flocculate of the algae cells are convenient.
2. The carbon nitride modified nano Fe used in the invention3O4After the algae inhibiting process, the material can make flocculate settle and recover quickly under the condition of external magnetic field, and after washing, the material can be used for inhibiting algae for several timesAnd (6) carrying out the process. The method provides a more efficient and convenient recovery mode while achieving the same or higher algae inhibiting effect as the existing algae inhibiting process. And the recovered carbon nitride modified nano Fe3O4The material still has excellent algae inhibiting effect after being recycled for many times.
3. The invention uses nano Fe3O4And carbon nitride as raw materials, and the carbon nitride modified nano Fe is prepared by a series of mixing processes and then high-temperature calcination3O4Material, obtained carbon nitride modified nano Fe3O4Compared with the existing algae inhibiting process, the material can adsorb and flocculate algae in a short time to achieve an ideal algae inhibiting effect.
Drawings
FIG. 1 shows carbon nitride modified nano Fe with different mass ratios3O4Comparative plot of material against algal cell removal rate.
FIG. 2 shows carbon nitride modified nano Fe with a mass ratio of 1:33O4The chlorophyll a content of the material changes with time under different adding amounts.
FIG. 3 shows carbon nitride modified nano Fe with a mass ratio of 1:33O4And (5) a material recycling performance diagram.
Detailed Description
The invention is further described with reference to specific examples.
Example 1
Carbon nitride modified nano Fe3O4The preparation method of the material comprises the following specific steps:
placing the crucible filled with a proper amount of dicyandiamide in a box-type atmosphere furnace, heating to 500 ℃ at the heating rate of 10 ℃/min, calcining for 2h at 500 ℃, heating to 520 ℃ at the heating rate of 5 ℃/min, calcining for 2h at 520 ℃, and naturally cooling to room temperature to obtain the pure carbon nitride. Taking four parts of 1.0g of nano Fe3O4Respectively putting the mixture and 0.5 g, 1.0g, 3.0g and 5.0g of carbon nitride into a glass beaker, adding 50mL of absolute ethyl alcohol, uniformly stirring, and then carrying out ultrasonic treatment for 30 min. Drying the beaker filled with the mixture in a 60 ℃ oven for 12h, grinding uniformly, and sieving with a 60-mesh sieve to obtain uniform depthBrown solid powder. Adding a proper amount of the dark brown solid powder into a ceramic crucible, placing the ceramic crucible in a muffle furnace at 450 ℃ for calcining for 2h, and then cooling to room temperature to respectively obtain nano Fe3O4The mass ratio of the nano Fe to the carbon nitride is 2:1, 1:2, 1:3 and 1:53O4A material.
Example 2
Nano Fe modified by carbon nitride with different mass ratios3O4The material is subjected to an algae inhibition effect test, and the specific process is as follows:
step one, taking microcystis aeruginosa liquid cultured by BG11, adding a proper amount of algae liquid into a centrifuge tube, centrifuging at 3000rpm for 10min at room temperature, pouring out supernatant, adding ultrapure water, and preparing into algae suspension with a certain concentration. The resulting four algal suspensions were packed in four reactors, respectively.
Step two, four portions of 0.6g of carbon nitride modified nano Fe with different mass ratios (2: 1, 1:2, 1:3 and 1:5 respectively prepared in example 1)3O4The materials are respectively added into four 200mL algae suspensions, the magnetic stirring speed is set to be 300rpm, after 10min of reaction, a magnetic field is applied to the bottom of the reactor, and then the reactor is kept still for 10 min. Collecting supernatant as sample, measuring optical density chlorophyll a content of supernatant sample extracted from four algae suspensions, and determining carbon nitride modified nanometer Fe with each mass ratio3O4The material has a removal rate T to microcystis aeruginosa cells.
The microcystis aeruginosa cell removal rate T is obtained by calculating the chlorophyll a content of algae liquid before and after a measurement test, and the specific calculation formula is as follows:
wherein, C0Is the initial chlorophyll a content in the algae suspension; c1The chlorophyll a content of the algae suspension after reaction. Because the optical density chlorophyll a content of the microcystis aeruginosa is in positive correlation with the cell density (or biomass), the expression can accurately obtain the removal rate T of the microcystis aeruginosa cells.
Adding pure g-C3N4Pure nano Fe3O4Four carbon nitride modified nano Fe with different mass ratios3O4The comparison of the algae inhibiting effect of the material is shown in figure 1. As can be seen from FIG. 1, compared with the unmodified nano Fe3O4Pure g-C of3N4Nano Fe modified by carbon nitride3O4The material obviously increases the algae inhibiting effect of the material, wherein after the composite catalyst with the mass ratio of 1:3 reacts for 10min, the algae cell removal rate can reach 89%, the algae inhibiting effect is optimal, the composite catalyst is the optimal mass ratio, and the composite catalyst has obvious advantages compared with other mass ratios. Through preliminary analysis, the mass ratio of the carbon nitride modified nano Fe is 1:33O4The reason why the material has better algae inhibiting effect is that the material has stronger adsorption and magnetic flocculation capacity to algae cells under the mass ratio, and the algae cells in the solution are easily separated from water efficiently under the action of an external magnetic field.
Example 3
Carbon nitride modified nano Fe3O4The algae inhibition efficiency comparison test of the material under the conditions of different adding amounts and different treatment times comprises the following specific processes:
step one, taking microcystis aeruginosa liquid cultured by BG11, adding a proper amount of algae liquid into a centrifuge tube, centrifuging at 3000rpm for 10min at room temperature, pouring out supernatant, adding ultrapure water, and preparing into algae suspension with a certain concentration.
Step two, modifying nano Fe by carbon nitride with mass ratio of 1:33O4Materials four groups of algal inhibition tests were performed on the resulting algal suspension. In each group of algal inhibition experiments, the amount of the algal suspension was 200ml, and the magnetic stirring speed was set to 300 rpm. Carbon nitride modified nano Fe in four-group algae inhibition test3O4The addition amounts of the materials are respectively 0.5, 1.0, 3.0 and 5.0 g/L. In each group of algae inhibition tests, samples are taken when catalysts are added for 0min, 2 min, 5 min and 10min, the chlorophyll a content of the samples is measured, and the removal rate T of the microcystis aeruginosa cells is calculated respectively.
Carbon nitride modified nano Fe with mass ratio of 1:3 in each adding amount3O4Material pairThe time dependence of the corresponding algal cell removal rate is shown in FIG. 2. The result shows that when the adding amount of the composite catalyst is 3.0g/L, the algae cell removal rate can reach more than 89% after the reaction is carried out for 10 min.
Example 4
Carbon nitride modified nano Fe3O4The recycling property of the material is tested, and the specific process is as follows:
and circulating one: modifying nano Fe by using carbon nitride with the mass ratio of 3.0g/L being 1:33O4Adding the material into the algae suspension, magnetically stirring for 10min, standing for 10min under an external magnetic field, and measuring the algae cell removal rate of the sample.
And II, circulation: collecting flocculate of the material and the algae cells in the first circulation, washing the flocculate for several times by using ethanol and distilled water after the flocculate is subjected to the action of ultrasonic waves and an external magnetic field, adding the flocculate into the algae suspension under the same adding condition, and measuring the removal rate of the algae cells of the sample through the same reaction process.
And (3) circulation three: collecting flocculate of the material and the algae cells in the second circulation, washing for several times by using ethanol and distilled water after the action of ultrasonic waves and an external magnetic field, reacting again under the same condition, and determining the removal rate of the algae cells of the sample.
In the first to third cycles, the pretreatment method and the algae inhibiting conditions of the algae solution are the same as those in example 2.
FIG. 3 is 1:3 carbon nitride modified nano Fe3O4And (5) a material recycling performance diagram. The result shows that after three times of circulation, the removal rate of the catalyst to the algae cells is still as high as 80 percent, and the material is proved to have good recycling property.
Claims (10)
1. Carbon nitride modified nano Fe3O4The material is applied as an algae inhibitor.
2. Carbon nitride modified nano Fe of claim 13O4The application of the material in inhibiting algae is characterized in that: the carbon nitride modified nano Fe3O4In the material, nano Fe3O4Mass ratio to carbon nitride of 1:5~2:1。
3. Carbon nitride modified nano Fe of claim 13O4The application of the material in inhibiting algae is characterized in that: the carbon nitride modified nano Fe3O4In the material, nano Fe3O4And the mass ratio of carbon nitride is 1: 3.
4. An algae inhibiting method is characterized in that: modifying the carbon nitride of any one of claims 1 to 3 with nano Fe3O4The material was added to the treated algal solution and stirring was applied.
5. The algae-inhibiting method according to claim 1, wherein: the carbon nitride modified nano Fe3O4The amount of the material used is 1.0-5.0 g/L relative to the algae liquid to be treated.
6. The algae-inhibiting method according to claim 1, wherein: applying a magnetic field to the algae liquid to be treated; after the algae inhibiting treatment is finished, collecting flocculate settled under the action of a magnetic field; the obtained flocculate is cleaned and recycled to obtain reusable carbon nitride modified nano Fe3O4A material.
7. Carbon nitride modified nano Fe3O4The preparation method of the material is characterized by comprising the following steps: step one, mixing carbon nitride and nano Fe3O4Mixing; the mixing process comprises the operations of uniformly mixing, drying, grinding and sieving to obtain a solid mixture;
step two, calcining the solid mixture obtained in the step one, and cooling to room temperature to obtain the carbon nitride modified nano Fe3O4A material.
8. Carbon nitride modified nano Fe of claim 73O4The preparation method of the material is characterized by comprising the following steps: the nano Fe3O4And carbon nitrideThe mass ratio of (A) to (B) is 2: 1-1: 5.
9. Carbon nitride modified nano Fe of claim 73O4The preparation method of the material is characterized by comprising the following steps: the mixing method in the first step comprises the following steps: mixing nano Fe3O4Placing the mixture and carbon nitride in a preparation container, adding absolute ethyl alcohol, uniformly stirring, then carrying out ultrasonic treatment and drying treatment, and carrying out grinding and 60-mesh sieve screening to obtain a solid mixture in a dark brown powder shape.
10. Carbon nitride modified nano Fe of claim 73O4The preparation method of the material is characterized by comprising the following steps: calcining carbon nitride in the first step by using dicyandiamide as a precursor; the calcination conditions were: heating to 500 deg.C at a heating rate of 10 deg.C/min in a box-type atmosphere furnace, calcining at 500 deg.C for 2 hr, heating to 520 deg.C at a heating rate of 5 deg.C/min, calcining at 520 deg.C for 2 hr, and naturally cooling to room temperature; the calcination conditions in the second step are as follows: heating a muffle furnace to 450 ℃, putting the muffle furnace into a crucible containing the solid mixture obtained in the step one, calcining the mixture at 450 ℃ for 2 hours, and naturally cooling the calcined mixture to room temperature to obtain brown solid powdery carbon nitride modified nano Fe3O4A material.
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CN114751484A (en) * | 2022-05-12 | 2022-07-15 | 东北电力大学 | Alga removing method of ferroferric oxide photo-thermal nano material |
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