CN112774631B - Method for preparing biochar-based composite adsorption material from aquatic product processing waste and application of biochar-based composite adsorption material in antimony-containing wastewater treatment - Google Patents
Method for preparing biochar-based composite adsorption material from aquatic product processing waste and application of biochar-based composite adsorption material in antimony-containing wastewater treatment Download PDFInfo
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Abstract
A method for preparing a biochar-based composite adsorption material by utilizing aquatic product processing waste products and application of the biochar-based composite adsorption material in antimony-containing wastewater treatment relate to the field of combination of aquatic product processing waste product recovery treatment and antimony-containing wastewater treatment. The aquatic product processing waste product is subjected to acid dissolution, pH value adjustment, extraction, solid-liquid separation, washing and drying, so that the aquatic product processing waste product biochar material is obtained; dissolving the waste biochar material, tin chloride, copper nitrate and manganese nitrate in water and dilute nitric acid, stirring and mixing uniformly, and regulating the pH value of the system by using an ammonia water solution; transferring the reaction liquid into a heat-collecting type constant-temperature water bath magnetic stirring reactor for solvothermal reaction; and then drying to obtain the biochar-based composite adsorption material which can be used for the environmental treatment of the industrial domestic sewage and waste water and waste gas containing antimony (3-valent antimony and 5-valent antimony).
Description
Technical Field
The invention relates to the field of the combination of the recovery treatment of aquatic product processing waste products and the treatment of antimony-containing wastewater, in particular to a method for preparing a biochar-based composite adsorption material by utilizing the aquatic product processing waste products and application of the biochar-based composite adsorption material in the treatment of the antimony-containing wastewater.
Background
The biochar-based adsorption material has abundant porous structures, superhigh specific surface area and abundant surface functional groups, and is widely applied to the fields of adsorption separation, sewage treatment, gas purification and the like. Because of its unique three-dimensional structure, it is now widely focused, has a unique framework structure, a high surface area, a directional distribution of channels, and a high chemical stability.
Antimony pollution is the environmental pollution of antimony and its compounds. Antimony and antimony-containing metals smelting or coal mining, and other processes using antimony or compounds, can produce waste gases, waste water and waste residues containing antimony elements or compounds thereof to pollute the environment. During the combustion or smelting of minerals, antimony is introduced into the atmosphere in the form of vapors or dust. The antimony in the water is from the dissolution of antimony-containing rock, the discharge of antimony-containing industrial wastewater, and the rainfall containing antimony. Water permeates into the soil and also contaminates it. Enriching antimony in water to 3X 10 -6 When the algae is started to be poisoned, the algae can be killed to 12 multiplied by 10 -6 And is toxic to fish. The average antimony content in human body is 5.8 mg, and most of antimony is from tableware, ceramic glaze and the like. Workers engaged in mining and smelting antimony ores are prone to antimony poisoning. Contact stibium (Sb) 2 O 3 ) About half of the individuals have heart failure. Antimony is similar to arsenic, and trivalent antimony is more toxic than pentavalent antimony. Trivalent antimony (SbH) 3 ) Has strong toxicity, and can cause hemolysis, liver and kidney disorder and pulmonary edema after inhalation. The smoke generated in factories stimulates skin mucous membrane, causes dermatitis, rhinitis and upper respiratory tract inflammation, can cause tumors and is a cancerogenic suspicious substance.
The invention aims to prepare biochar by aquatic product processing waste products and load a multi-element composite filler so as to realize effective treatment of antimony-containing wastewater.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for preparing a biochar-based composite adsorption material by utilizing aquatic product processing waste products and application of the method in antimony-containing wastewater treatment.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: a method for preparing a biochar-based composite adsorption material by utilizing aquatic product processing waste products comprises the following steps:
(1) preparation of waste biochar material for aquatic product processing
The aquatic product processing waste product is subjected to acid dissolution, pH value adjustment, extraction, solid-liquid separation, washing and drying, so that the aquatic product processing waste product biochar material is obtained;
the aquatic product processing waste is selected from one of the skin, scale and shell of fish, shrimp and crab;
(2) preparation of biochar-based composite adsorption material
Dissolving the waste biochar material, tin chloride, copper nitrate and manganese nitrate in water and dilute nitric acid, stirring and mixing uniformly, and regulating the pH value of the system to 5-11 by using an ammonia water solution;
transferring the reaction liquid into a heat-collecting type constant-temperature water bath magnetic stirring reactor, starting 1000r/min rotating speed magnetic stirring, and carrying out solvothermal reaction for 90 minutes at the temperature of 75 ℃ by hydrothermal impregnation;
then closing the magnetic stirring and heating functions, transferring into a baking oven, setting the baking temperature to be 110 ℃, and drying for 120 minutes to obtain the biochar-based composite adsorption material CuO-SnO 2 -MnO 2 。
Preferably, the weight ratio of the waste biochar material in the finally prepared biochar-based composite adsorption material is 60-80%, and the filler is CuO-SnO 2 -MnO 2 The weight ratio of the components is 20-40%.
Preferably, the finally prepared biochar-based composite adsorption material contains CuO and SnO 2 And MnO 2 The molar ratio of (2) is 1:1:1.
preferably, the prepared biochar-based composite adsorption material has a mixed structure in a spherical shape and a rod shape, the pore canal structure is obvious, the microstructure presents multiple stages and multiple dimensions, and the size range of the porous structure is between 200nm and 1 um.
The invention also provides application of the biochar-based composite adsorption material in antimony-containing wastewater treatment.
Compared with the prior art, the invention has the beneficial effects that:
the invention takes the treated waste of the aquatic plant with high activity as the main carrier, and takes CuO-SnO with certain content and composition 2 -MnO 2 As filler of the adsorption material, the magnetic stirring solvothermal method is used for preparing the multi-element composite adsorption material with excellent performance. Adopting an instrument characterization means XRD and SEM to characterize the structure of the material, testing the adsorption performance, and screening out the biochar-based composite adsorption material CuO-SnO with excellent performance 2 -MnO 2 . The adsorption capacity, the removal time and the material composition of the biological carbon-based composite material with high activity on the sewage solution containing antimony (3-valent antimony and 5-valent antimony) of the serial aquatic plant wastes with different compositions can be seen. With (30%) CuO-SnO 2 -MnO 2 The modified aquatic plant waste has the best high-activity biochar-based (70%) adsorption effect, and the adsorption amount reaches 205mg/g. The prepared target product achieves the expected target of experimental design, and the CuO-SnO is proved 2 -MnO 2 The modified biochar-based adsorption material with high activity for the aquatic product factory waste treated by the process can be used for environmental treatment of industrial domestic sewage and waste water and waste gas containing antimony (3-valent antimony and 5-valent antimony), and the enriched antimony is used for industrial production fields of fire retardants, electronic products, alloys, pigments, ceramics, chemical industry, synthetic fibers, building materials, medicines and the like, so that the recycling of antimony resources is facilitated, the environment is protected, and the resources and the energy are saved.
Drawings
The method for preparing the biochar-based composite adsorbing material by utilizing the aquatic product processing waste product and the application of the biochar-based composite adsorbing material in the antimony-containing wastewater treatment are further described below with reference to the examples and the accompanying drawings.
FIG. 1 is an XRD pattern for each series of composite adsorbent materials prepared in examples 1-10.
FIG. 2 is a graph showing the percentage of antimony ions adsorbed by each of the series of composite adsorbent materials prepared in examples 1 to 10.
FIG. 3 is a graph showing the adsorption amounts of the composite adsorbents of examples 1 to 10.
Fig. 4 is a low, medium, and high magnification SEM image of the composite adsorbent material prepared in example 1 in sequence.
Detailed Description
Example 1
In the implementation, the prepared biochar-based composite adsorption material C-CuO-SnO 2 -MnO 2 In the method, the weight ratio of the biochar material in the finally prepared biochar-based composite adsorption material is 70 percent, and the biochar material is CuO-SnO serving as a filler 2 -MnO 2 The weight ratio is 30%. Finally prepared biocharCuO and SnO in base composite adsorption material 2 And MnO 2 The molar ratio of (2) is 1:1:1. the preparation method comprises the following steps:
(1) preparation of waste biochar material for aquatic product processing
The aquatic product processing waste product is subjected to acid dissolution, pH value adjustment, extraction, solid-liquid separation, washing and drying, so that the aquatic product processing waste product biochar material is obtained;
the aquatic product processing waste is selected from one of the skin, scale and shell of fish, shrimp and crab;
(2) preparation of biochar-based composite adsorption material
Dissolving the waste biochar material, tin chloride, copper nitrate and manganese nitrate in water and dilute nitric acid, stirring and mixing uniformly, and regulating the pH value of the system to 5-11 by using an ammonia water solution;
transferring the reaction liquid into a heat-collecting type constant-temperature water bath magnetic stirring reactor, starting 1000r/min rotating speed magnetic stirring, and carrying out solvothermal reaction for 90 minutes at the temperature of 75 ℃ by hydrothermal impregnation;
then closing the magnetic stirring and heating functions, transferring into a baking oven, setting the baking temperature to be 110 ℃, and drying for 120 minutes to obtain the biochar-based composite adsorption material CuO-SnO 2 -MnO 2 (1：1：1)。
Example 2
In the implementation, the prepared biochar-based composite adsorption material C-CuO-SnO 2 -MnO 2 In the method, the weight ratio of the biochar material in the finally prepared biochar-based composite adsorption material is 70 percent, and the biochar material is CuO-SnO serving as a filler 2 -MnO 2 The weight ratio is 30%. CuO and SnO in finally prepared biochar-based composite adsorption material 2 And MnO 2 The molar ratio of (2) is 1:2:2. the preparation method is the same as in example 1, and the biochar-based composite adsorption material C-CuO-SnO is obtained 2 -MnO 2 (1：2：2)。
Example 3
In the implementation, the prepared biochar-based composite adsorption material C-CuO-SnO 2 -MnO 2 In the method, the biochar material is subjected to final preparation of biochar-based composite adsorptionThe material accounts for 70 percent of the weight of the material, and the filler is CuO-SnO 2 -MnO 2 The weight ratio is 30%. CuO and SnO in finally prepared biochar-based composite adsorption material 2 And MnO 2 The molar ratio of (2): 1:1. the preparation method is the same as in example 1, and the biochar-based composite adsorption material C-CuO-SnO is obtained 2 -MnO 2 (2：1：1)。
Example 4
In the implementation, the prepared biochar-based composite adsorption material C-CuO-SnO 2 -MnO 2 In the method, the weight ratio of the biochar material in the finally prepared biochar-based composite adsorption material is 70 percent, and the biochar material is CuO-SnO serving as a filler 2 -MnO 2 The weight ratio is 30%. CuO and SnO in finally prepared biochar-based composite adsorption material 2 And MnO 2 The molar ratio of (2): 1:2. the preparation method is the same as in example 1, and the biochar-based composite adsorption material C-CuO-SnO is obtained 2 -MnO 2 (2：1：2)。
Example 5
In the implementation, the prepared biochar-based composite adsorption material C-CuO-SnO 2 -MnO 2 In the method, the weight ratio of the biochar material in the finally prepared biochar-based composite adsorption material is 70 percent, and the biochar material is CuO-SnO serving as a filler 2 -MnO 2 The weight ratio is 30%. CuO and SnO in finally prepared biochar-based composite adsorption material 2 And MnO 2 The molar ratio of (2): 2:1. the preparation method is the same as in example 1, and the biochar-based composite adsorption material C-CuO-SnO is obtained 2 -MnO 2 (2：2：1)。
Example 6
In the implementation, the prepared biochar-based composite adsorption material C-CuO-SnO 2 -MnO 2 In the method, the weight ratio of the biochar material in the finally prepared biochar-based composite adsorption material is 70 percent, and the biochar material is CuO-SnO serving as a filler 2 -MnO 2 The weight ratio is 30%. CuO and SnO in finally prepared biochar-based composite adsorption material 2 And MnO 2 The molar ratio of (2) is 1:1:2. the preparation method is the same as in example 1, and the biochar-based composite adsorption material C-CuO-SnO is obtained 2 -MnO 2 (1：1：2)。
Example 7
In the implementation, the prepared biochar-based composite adsorption material C-CuO-SnO 2 -MnO 2 In the method, the weight ratio of the biochar material in the finally prepared biochar-based composite adsorption material is 70 percent, and the biochar material is CuO-SnO serving as a filler 2 -MnO 2 The weight ratio is 30%. CuO and SnO in finally prepared biochar-based composite adsorption material 2 And MnO 2 The molar ratio of (2) is 1:2:1. the preparation method is the same as in example 1, and the biochar-based composite adsorption material C-CuO-SnO is obtained 2 -MnO 2 (1：2：1)。
Example 8
In this embodiment, the preparation method is the same as in example 1, except that tin chloride and copper nitrate are not added to obtain biochar-based composite adsorption material C-MnO 2 。
Example 9
In this embodiment, the preparation method is the same as in example 1, except that copper nitrate and manganese nitrate are not added to obtain the biochar-based composite adsorption material C-SnO 2 。
Example 10
In this embodiment, the preparation method is the same as in example 1, except that tin chloride and manganese nitrate are not added, and the biochar-based composite adsorption material C-CuO is obtained.
FIG. 1 is an XRD pattern for each series of composite adsorbent materials prepared in examples 1-10. As can be seen from FIG. 1, the XRD diffraction pattern has a remarkable CuO, mnO 2 ，SnO 2 The diffraction peaks of the catalyst are relatively sharp, which indicates that the synthesized composite adsorbent is phase-matched with the experimental design target object C-CuO-SnO 2 -MnO 2 And are matched.
FIG. 2 shows the effect of the charcoal-based composite adsorbent materials of examples 1-10, prepared with different compositions, on the removal rate of the wastewater solution containing antimony (3-valent antimony and 5-valent antimony) under sunlight conditions. Wherein, the dosage of the sample adsorption material is 50mg, the adsorption time is 70min, the volume of the sewage solution containing antimony (3-valent antimony and 5-valent antimony) is 120mL, and the initial concentration is 100mg/L. As can be seen from FIG. 3, the implementationThe biochar-based composite adsorption material CuO-SnO prepared in example 1 2 -MnO 2 The adsorption effect of (1:1:1) is best, the removal rate reaches 99.4%, and the adsorption removal effect is better when all series products with different compositions are prolonged with time.
FIG. 3 is a graph showing adsorption capacity, removal time and material composition of the biochar-based composite material with high activity on antimony-containing (3-valent antimony and 5-valent antimony) solution prepared by the aquatic plant waste treated by the process in the series of examples 1 to 10 with different compositions under sunlight conditions. Wherein, the dosage of the sample adsorption material is 40mg, the adsorption time is 140min, and the volume of the solution containing antimony (3-valent antimony and 5-valent antimony) is 400mL. As can be seen from FIG. 4, the biochar-based composite adsorption material CuO-SnO prepared in example 1 2 -MnO 2 The adsorption effect (1:1:1) is best, the adsorption quantity reaches 205mg/g, the better the adsorption removal effect is when the series products with different compositions are prolonged along with time, the adsorption quantity is basically stable along with the increase of time after the adsorption time reaches 60 minutes, and the adsorption process is mainly completed within 60 minutes and the adsorption effect is good.
Experiments show that the prepared target product achieves the expected target of experimental design, and the prepared biochar-based composite adsorption material CuO-SnO is proved 2 -MnO 2 The method can be used for the environmental treatment of industrial sewage and wastewater containing antimony (3-valent antimony and 5-valent antimony) heavy metal solution, enriches antimony, and saves the fields of flame retardants, electronic products, alloys, pigments, ceramics, chemical industry, synthetic fibers, building materials, medicines and the like, is convenient for recycling antimony resources, protects the environment and saves resources and energy.
Fig. 4 is a low, medium, and high magnification SEM image of the composite adsorbent material prepared in example 1 in sequence. As can be seen from fig. 4, the prepared product has a mixed structure of a ball shape and a rod shape, and the pore canal structure is obvious, so that the product can be applied to wastewater adsorption treatment. And the microstructure of the composite material presents multiple stages and multiple dimensions, and the size range is between 200nm and 1 um.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.
Claims (1)
1. The application of the biochar-based composite adsorbing material prepared from the aquatic product processing waste in the treatment of the antimony-containing wastewater is characterized in that the preparation method of the biochar-based composite adsorbing material comprises the following steps:
(1) preparation of waste biochar material for aquatic product processing
The aquatic product processing waste product is subjected to acid dissolution, pH value adjustment, extraction, solid-liquid separation, washing and drying, so that the aquatic product processing waste product biochar material is obtained;
the aquatic product processing waste is selected from one of the skin, scale and shell of fish, shrimp and crab;
(2) preparation of biochar-based composite adsorption material
Dissolving the waste biochar material, tin chloride, copper nitrate and manganese nitrate in water and dilute nitric acid, stirring and mixing uniformly, and regulating the pH value of the system to 5-11 by using an ammonia water solution;
transferring the reaction liquid into a heat-collecting type constant-temperature water bath magnetic stirring reactor, starting 1000r/min rotating speed magnetic stirring, and carrying out solvothermal reaction for 90 minutes at the temperature of 75 ℃ by hydrothermal impregnation;
then closing the magnetic stirring and heating functions, transferring into a baking oven, setting the baking temperature to be 110 ℃, and drying for 120 minutes to obtain the biochar-based composite adsorption material CuO-SnO 2 -MnO 2 The method comprises the steps of carrying out a first treatment on the surface of the Wherein the weight ratio of the biochar material in the finally prepared biochar-based composite adsorption material is 70%, and the biochar material is CuO-SnO serving as a filler 2 -MnO 2 The weight ratio is 30%; cuO and SnO in biochar-based composite adsorption material 2 And MnO 2 The molar ratio of (2) is 1:1:1.
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| CN107413296A (en) * | 2017-07-21 | 2017-12-01 | 浙江省农业科学院 | A kind of charcoal ferrojacobsite composite for being used to adsorb heavy metal antimony cadmium |
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| CN105771899B (en) * | 2016-04-28 | 2019-02-26 | 农业部沼气科学研究所 | A kind of charcoal of efficient dephosphorization removing heavy metals, preparation method and applications |
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| CN107413296A (en) * | 2017-07-21 | 2017-12-01 | 浙江省农业科学院 | A kind of charcoal ferrojacobsite composite for being used to adsorb heavy metal antimony cadmium |
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