CN110548483A - preparation method and application of biochar/nano ferroferric oxide composite material - Google Patents
preparation method and application of biochar/nano ferroferric oxide composite material Download PDFInfo
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- CN110548483A CN110548483A CN201910442498.XA CN201910442498A CN110548483A CN 110548483 A CN110548483 A CN 110548483A CN 201910442498 A CN201910442498 A CN 201910442498A CN 110548483 A CN110548483 A CN 110548483A
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- ferroferric oxide
- nano ferroferric
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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
- B01J20/048—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 containing phosphorus, e.g. phosphates, apatites, hydroxyapatites
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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
- B01J20/20—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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- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention relates to a preparation method and application of a biochar/nano ferroferric oxide composite material, belonging to the field of material and environmental science and technology. Preparing a nano ferroferric oxide precursor by using a solution combustion synthesis method, adding the nano ferroferric oxide precursor into a suspension of a biomass raw material, and performing ultrasonic pyrolysis on a biochar/ferroferric oxide precursor compound to obtain the biochar/nano ferroferric oxide composite material. According to the invention, a solution combustion method is utilized for the first time, nano ferroferric oxide is generated on the biochar through a pyrolysis condition, the traditional coprecipitation method is replaced, the preparation method is simple, and the prepared biochar/nano ferroferric oxide composite material has high specific surface area and activity and has potential application value in the fields of environment and the like. Adsorption experiments prove that the biochar/nano ferroferric oxide composite material has a high antimony removal effect in a wide pH range.
Description
Technical Field
The invention belongs to the field of environment repairing materials, and particularly relates to a biochar/nano ferroferric oxide composite material.
Background
The nanoscale ferroferric oxide not only has the quantum size effect, the surface effect, the small-size effect and the macroscopic quantum tunneling effect, but also has special magnetic property, high thermodynamic stability, multiple functionality and excellent environmental compatibility. The method has good application prospect in the field of biotechnology and medicine, and also shows very wide application prospect in the field of environment.
Currently, many methods are used to prepare the ferroferric oxide nanostructure, such as chemical coprecipitation method, hydrothermal method, microemulsion method, sol method, etc. However, these methods suffer from more or less limitations, such as longer preparation times, low yields, less than ideal pore characteristics, and the like. In recent years, the solution combustion synthesis method has achieved great success in the preparation of nanomaterials, and chinese patent publication No. CN105312070B discloses a method for preparing a tungsten carbide supported platinum catalyst by solution combustion synthesis. However, the solution combustion synthesis method is not applied to the preparation of the nano ferroferric oxide at present. The invention prepares nano ferroferric oxide by using a solution combustion method, combines a biochar technology with a ferroferric oxide nano structure to prepare a biochar/ferroferric oxide nano composite material, and applies the biochar/ferroferric oxide nano composite material to remove antimony in a water body.
Disclosure of Invention
The invention aims to provide a preparation method of a biochar/nano ferroferric oxide composite material, which has the advantages of simple process, easy operation and convenient control of the ferroferric oxide content. The method comprises the following specific steps:
(1) Dissolving raw materials of an oxidant, namely ferric nitrate, an organic fuel and a combustion improver in a certain molar ratio into 200ml of deionized water, fully stirring, and preparing a uniform initial solution at room temperature;
(2) Pouring the prepared solution into a 1000ml beaker, heating the beaker on a temperature-controlled electric heating furnace, generating smoldering reaction after the solution is evaporated, and generating a precursor TC when the reaction is finished;
(3) Soaking the treated sunflower straws and a precursor TC in distilled water according to a proper mass ratio, and drying after ultrasonic treatment;
(4) and (4) putting the dried product in the step (3) into a tubular furnace for pyrolysis, and washing the pyrolysis product with deionized water to obtain the nano ferroferric oxide.
Further, in the step 1), the organic fuel is one or two of urea, citric acid and glycine.
further, in the step 1), the combustion improver is one or two of glucose and starch.
Further, in the step 1), the molar ratio of the oxidant ferric nitrate, the organic fuel and the combustion improver raw material in a certain molar ratio is 1: 2: 2-1: 3: 3.
Further, in the step 3), the straw is treated in a manner that the outer surface of the straw is removed and the straw is crushed into small particles.
Further, in the step 3), the mass ratio is 5: 1.
further, the pyrolysis condition in the step 3) is pyrolysis at 600 ℃ for 1 hour in a flowing N2 environment at a heating rate of 6 ℃/min.
The invention has the beneficial effects that:
the invention provides a preparation method of a biochar/nano ferroferric oxide composite material, under the method provided by the invention, the content of nano ferroferric oxide in the composite material has good controllability, and the content of nano ferroferric oxide in the composite material is in a simple multiple relation with the addition.
drawings
FIG. 1 is an XRD (X-ray diffraction) pattern of a biochar/nano ferroferric oxide composite material prepared in example 1;
FIG. 2 is a schematic diagram of the removal rate of antimony in water treated by the biochar/nano ferroferric oxide composite material according to different embodiments of application tests.
Detailed Description
the technical contents of the present invention will be further clarified by the following specific examples, but the contents of the present invention are not limited to the following examples.
Example 1
A biochar/nano ferroferric oxide composite material is prepared by the following steps:
(1) Mixing a mixture of 1: 2: 2 ferric nitrate (oxidant), glycine (organic fuel) and glucose (combustion improver) are dissolved in 200ml of deionized water and fully stirred to prepare a uniform initial solution at room temperature;
(2) Pouring the prepared solution into a 1000ml beaker, heating the beaker on a temperature-controlled electric heating furnace, generating smoldering reaction after the solution is evaporated, and terminating the reaction to generate a precursor TC;
(3) sunflower straw is subjected to outer skin removal, crushed into small particles, and mixed with a precursor TC according to the ratio of 10: 1, soaking the mixture in distilled water, performing ultrasonic treatment for 1 hour, and drying;
(4) and (4) putting the dried product in the step (3) into a tube furnace, and pyrolyzing the product at 600 ℃ for 1 hour in a flowing N2 environment at the heating rate of 6 ℃/min. And washing the pyrolysis product with deionized water to obtain the biochar/nano ferroferric oxide composite material. Is marked as C/Fe3O 4-1.
An XRD electron microscope image of the biochar/nano ferroferric oxide composite material prepared in the example 1 is shown in a figure 1.
Example 2
a preparation method of a hydroxyapatite modified biochar material comprises the following steps:
(1) Mixing a mixture of 1: 3: 3 ferric nitrate (oxidant), urea (organic fuel) and glucose (combustion improver) are dissolved in 200ml of deionized water and fully stirred, and a uniform initial solution is prepared at room temperature;
(2) Pouring the prepared solution into a 1000ml beaker, heating the beaker on a temperature-controlled electric heating furnace, generating smoldering reaction after the solution is evaporated, and terminating the reaction to generate a precursor TC;
(3) Sunflower straw is subjected to outer skin removal, crushed into small particles, and mixed with a precursor TC according to the ratio of 10: 1, soaking the mixture in distilled water, performing ultrasonic treatment for 1 hour, and drying;
(4) and (4) putting the dried product in the step (3) into a tube furnace, and pyrolyzing the product at 600 ℃ for 1 hour in a flowing N2 environment at the heating rate of 6 ℃/min. And washing the pyrolysis product with deionized water to obtain the biochar/nano ferroferric oxide composite material. Is marked as C/Fe3O 4-2.
Example 3
A preparation method of a hydroxyapatite modified biochar material comprises the following steps:
(1) mixing a mixture of 1: 3: 2, dissolving ferric nitrate (oxidant), citric acid (organic fuel) and starch (combustion improver) in 200ml of deionized water, fully stirring, and preparing a uniform initial solution at room temperature;
(2) pouring the prepared solution into a 1000ml beaker, heating the beaker on a temperature-controlled electric heating furnace, generating smoldering reaction after the solution is evaporated, and terminating the reaction to generate a precursor TC;
(3) Sunflower straw is subjected to outer skin removal, crushed into small particles, and mixed with a precursor TC according to the ratio of 10: 1, soaking the mixture in distilled water, performing ultrasonic treatment for 1 hour, and drying;
(4) And (4) putting the dried product in the step (3) into a tube furnace, and pyrolyzing the product at 600 ℃ for 1 hour in a flowing N2 environment at the heating rate of 6 ℃/min. And washing the pyrolysis product with deionized water to obtain the biochar/nano ferroferric oxide composite material. Is marked as C/Fe3O 4-3.
example 4
The biochar/nano ferroferric oxide composite material prepared in the embodiment 1-3 is used for testing the adsorption performance of heavy metal antimony in water. The test method comprises the following steps: 0.1 g of the prepared biochar/nano ferroferric oxide composite material is weighed and respectively added into 50mL of antimony (III) solution with the initial concentration of 50 mg/L and the initial p H of 2, 3, 4, 5, 6, 7 and 8, the oscillation is carried out at room temperature, the sampling is carried out after 12h, and the ICP-MS is used for measuring the residual concentration of the antimony (III) in the solution. The results are shown in FIG. 2. The detection result shows that the biochar/nano ferroferric oxide composite material can effectively remove antimony in water, the C/Fe3O4-1 has the best removal effect, and the antimony removal rate is better in a wider pH range.
Claims (8)
1. A preparation method and application of a biochar/nano ferroferric oxide composite material are characterized in that the preparation method comprises the following steps:
(1) Dissolving raw materials of an oxidant, namely ferric nitrate, an organic fuel and a combustion improver in a certain molar ratio into 200ml of deionized water, fully stirring, and preparing a uniform initial solution at room temperature;
(2) pouring the prepared solution into a 1000ml beaker, heating the beaker on a temperature-controlled electric heating furnace, generating smoldering reaction after the solution is evaporated, and generating a precursor TC when the reaction is finished;
(3) Soaking the treated sunflower straws and a precursor TC in distilled water according to a proper mass ratio, and drying after ultrasonic treatment;
(4) and (4) putting the dried product in the step (3) into a tubular furnace for pyrolysis, and washing the pyrolysis product with deionized water to obtain the nano ferroferric oxide.
2. the preparation method of nano ferroferric oxide according to claim 1, characterized by comprising the following steps: in the step 1), the organic fuel is one or two of urea, citric acid and glycine.
3. The preparation method of nano ferroferric oxide according to claim 1, characterized by comprising the following steps: in the step 1), the combustion improver is one or two of glucose and starch.
4. The preparation method of nano ferroferric oxide according to claim 1, characterized by comprising the following steps: in the step 1), the molar ratio of the oxidant ferric nitrate, the organic fuel and the combustion improver raw material in a certain molar ratio is 1: 2: 2-1: 3: 3.
5. The preparation method of nano ferroferric oxide according to claim 1, characterized by comprising the following steps: in the step 3), the straw treatment mode is to remove the outer surface of the straw and crush the straw into small particles.
6. the preparation method of nano ferroferric oxide according to claim 1, characterized by comprising the following steps: in the step 3), the mass ratio is 5: 1.
7. the preparation method of nano ferroferric oxide according to claim 1, characterized by comprising the following steps: the pyrolysis condition in the step 3) is that pyrolysis is carried out for 1 hour at 600 ℃ at the temperature rise rate of 6 ℃/min in the flowing N2 environment.
8. The application of the biochar/nano ferroferric oxide composite material in the prevention and treatment of heavy metal pollution in water as claimed in claim 1.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111203180A (en) * | 2020-01-15 | 2020-05-29 | 浙江大学 | Magnetic biochar composite adsorbent and preparation method and application thereof |
| CN113281573A (en) * | 2021-05-21 | 2021-08-20 | 哈尔滨理工大学 | Method for testing electromagnetic performance of nano ferroferric oxide |
| CN113289584A (en) * | 2021-07-05 | 2021-08-24 | 黑龙江省科学院高技术研究院 | Preparation method and application of sunflower straw charcoal adsorbent |
| CN117417525A (en) * | 2023-10-23 | 2024-01-19 | 西安工程大学 | Poly-N-phenylglycine@biochar composite material and preparation method and application thereof |
| CN117417525B (en) * | 2023-10-23 | 2024-04-19 | 西安工程大学 | Poly-N-phenylglycine@biochar composite material and preparation method and application thereof |
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| WO2014018653A1 (en) * | 2012-07-24 | 2014-01-30 | Kansas State University Research Foundation | Nanoparticle catalyst capable of forming aromatic hydrocarbons from co2 and h2 |
| CN105271431A (en) * | 2015-10-12 | 2016-01-27 | 南京大学 | Method for preparing ferriferrous oxide magnetic material and composite material thereof |
| CN105753608A (en) * | 2016-05-17 | 2016-07-13 | 北京化工大学 | Preparation method and application of novel iron-based biochar |
| CN105879834A (en) * | 2014-10-21 | 2016-08-24 | 王欣 | Preparation method of adsorbent for removing phosphorus and heavy metal anions in water as well as application method |
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2019
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Patent Citations (5)
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| WO2014018653A1 (en) * | 2012-07-24 | 2014-01-30 | Kansas State University Research Foundation | Nanoparticle catalyst capable of forming aromatic hydrocarbons from co2 and h2 |
| CN103316636A (en) * | 2013-07-05 | 2013-09-25 | 河南农业大学 | Method for preparing biomass-based magnetic activated carbon |
| CN105879834A (en) * | 2014-10-21 | 2016-08-24 | 王欣 | Preparation method of adsorbent for removing phosphorus and heavy metal anions in water as well as application method |
| CN105271431A (en) * | 2015-10-12 | 2016-01-27 | 南京大学 | Method for preparing ferriferrous oxide magnetic material and composite material thereof |
| CN105753608A (en) * | 2016-05-17 | 2016-07-13 | 北京化工大学 | Preparation method and application of novel iron-based biochar |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111203180A (en) * | 2020-01-15 | 2020-05-29 | 浙江大学 | Magnetic biochar composite adsorbent and preparation method and application thereof |
| CN111203180B (en) * | 2020-01-15 | 2021-06-11 | 浙江大学 | Magnetic biochar composite adsorbent and preparation method and application thereof |
| CN113281573A (en) * | 2021-05-21 | 2021-08-20 | 哈尔滨理工大学 | Method for testing electromagnetic performance of nano ferroferric oxide |
| CN113289584A (en) * | 2021-07-05 | 2021-08-24 | 黑龙江省科学院高技术研究院 | Preparation method and application of sunflower straw charcoal adsorbent |
| CN117417525A (en) * | 2023-10-23 | 2024-01-19 | 西安工程大学 | Poly-N-phenylglycine@biochar composite material and preparation method and application thereof |
| CN117417525B (en) * | 2023-10-23 | 2024-04-19 | 西安工程大学 | Poly-N-phenylglycine@biochar composite material and preparation method and application thereof |
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Application publication date: 20191210 |