Preparation method of iron source adsorbed doped material

By using high-frequency ultrasonic modification, low-frequency ultrasonic magnetization, and multi-heat source solidification treatment, iron ions in industrial iron waste liquid are converted into nano-iron oxide particles and fixed in porous carbon materials. This solves the problem of difficult post-treatment of iron ions adsorbed by biochar and realizes efficient utilization and energy storage applications.

CN117654457BActive Publication Date: 2026-02-13CHINA JILIANG UNIV +1
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Patent Information

Application Number
CN202311355019.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-10-19
Publication Date
2026-02-13
Estimated Expiration
2043-10-19

AI Technical Summary

Technical Problem

In existing technologies, biochar adsorbs iron ions, which is difficult to process and regenerate, leading to environmental risks and resource waste. At the same time, the application scope of biochar is limited.

Method used

By using high-frequency ultrasonic modification, low-frequency ultrasonic magnetization, and multi-heat source curing treatment, iron ions in industrial iron waste liquid are converted into nano-iron oxide particles and fixed in a porous carbon material structure to form an iron source adsorption doping material, thereby achieving efficient utilization.

Benefits of technology

This method achieves efficient fixation and stability of iron ions, improves the thermal stability and reusability of materials, and expands the application of biochar in energy storage technology.

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Abstract

The application discloses a preparation method of an iron source adsorption doped material, which can convert iron ions in industrial iron waste liquid into nano iron oxide particles and fix the nano iron oxide particles in a porous carbon material structure, realizes efficient utilization of waste metals, reduces energy consumption, improves heating efficiency and realizes uniform heating by using ultrasonic and multi-heat source methods, reduces compounds generated due to activated biochar, solves industrial wastewater pollution problems, solves waste metal recycling problems and realizes energy storage application of the solidified material.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of electric energy storage doped materials, in particular to the technical field of a preparation method of iron source adsorption doped materials. BACKGROUND

[0002] Carbon-based materials are the earliest applied, most mature and most widely used electrode materials. Compared with other carbon materials with complex preparation process and high cost, porous activated carbon prepared from biochar has the advantages of low cost, large specific surface area, rich pore structure and stable physical and chemical properties, and is widely used in water pollutant adsorption and electrode materials.

[0003] Industrial wastewater pollution refers to the phenomenon that harmful substances, pollutants or high-concentration wastewater generated in the industrial production process are discharged or leaked into the water environment, causing adverse effects on water quality. In order to protect water resources and maintain environmental sustainable development, the treatment and management of industrial wastewater become crucial. Iron ions are one of the common industrial wastewater pollutants. When there are too many iron ions in water, not only will it cause serious damage to the water and soil environment, but also will lead to the waste of this indispensable natural resource. The existing treatment methods for metal pollution include photocatalysis, flotation, chemical precipitation, ion exchange, electrochemical treatment, membrane separation and adsorption. Among them, the adsorption method is one of the most effective methods for treating industrial wastewater pollution at present due to its simple process and high removal rate. The adsorption method can use biochar as an adsorbent, and the adsorbed iron ions exist in the pores of the biochar in the form of molecules, ions or functional groups, and interact with the biochar through van der Waals force, electrostatic force, dispersion force or chemical bond force. However, biochar enriched with iron elements is difficult to handle, and direct use in land may pose potential risks to the environment, and the regeneration of biochar also faces certain difficulties. SUMMARY

[0004] The purpose of the present application is to solve the problems in the prior art and provide a preparation method of iron source adsorption doped materials, which can convert iron ions in industrial iron waste liquid into nano iron oxide particles and fix them in the structure of porous carbon materials, realizing efficient utilization of waste metals. By using ultrasonic and multi-heat source methods, energy consumption can be reduced, heating efficiency can be improved, and uniform heating can be realized. The compounds generated by activating biochar can be reduced, the problems of industrial wastewater pollution and waste metal recycling can be solved, and the energy storage application of the solidified material can be realized.

[0005] To achieve the above purpose, the present application provides a preparation method of iron source adsorption doped materials, comprising the following steps:

[0006] a) high-frequency ultrasonic modification: the biochar material prepared after pyrolysis of waste biomass is subjected to high-frequency ultrasonic modification treatment, and after filtration, the ultrasonically modified biochar material is obtained, the ultrasonically modified biochar material is used as a substrate, industrial iron waste liquid is used as an iron source, the ultrasonically modified biochar material and the industrial iron waste liquid are mixed, and a solid-liquid mixture is obtained;

[0007] b) low-frequency ultrasonic magnetization treatment: the solid-liquid mixture prepared in step a) is subjected to intermittent ultrasonic oscillation adsorption, then hydrogen peroxide solution is added and an electromagnetic coil is energized, after reaction for 0.5-1 h, filtration is performed, then the adsorbent material is obtained after multiple washing to remove waste metal liquid and drying;

[0008] c) confined multi-heat source solidification loading: the adsorbent material prepared in step b) is uniformly placed in a specially designed dispersed carrier, and subjected to resistance wire-electromagnetic multi-heat source solidification loading treatment, initially heated by resistance wire heating and electromagnetic heating, after reaching the specified temperature for 5 min, the resistance wire heating is turned off, and the solidification loading temperature is maintained for a period of time for solidification, and then cooled to obtain the finished product.

[0009] As preferred, in step a), the ultrasonic frequency of the high-frequency ultrasonic modification is 80-200 kHz, the ultrasonic time is 1-3 h, and the ultrasonic temperature is 70-100℃.

[0010] As preferred, in step b), the ultrasonic frequency of the low-frequency ultrasonic magnetization treatment is 30-60 kHz, the ultrasonic intermittent is 3 min of ultrasonic treatment every 15 min, the ultrasonic temperature is 20-40℃, the adsorption time is 12-48 h, the concentration of hydrogen peroxide is not less than 3%, the magnetization coil is a solenoid magnetic field generating coil, and the central magnetic field is not less than 300 GS.

[0011] As preferred, in step a), the iron ion concentration of the industrial iron waste liquid is not less than 0.1 g / L.

[0012] As preferred, the industrial iron waste liquid includes ferrous ion-containing organic liquid phase pollutants, iron ion-containing organic liquid phase pollutants, and iron ion-containing inorganic liquid phase pollutants, the iron ion-containing organic liquid phase pollutants contain any one or several of C6H 10 FeO6, Fe(C5H5)2, FeC6H5O7, and Fe[C2H4O2N]2, the iron ion-containing inorganic liquid phase pollutants are iron salts and iron complexes, etc., and the iron ion-containing inorganic liquid phase pollutants contain any one or several of FeCl2, FeCl3, FeSO4, Fe2(SO4)3, K4[Fe(CN)6], and [Fe(SCN) n ] 3-n .

[0013] As preferred, in step c), the multi-heat source solidification load heating method is a combination of resistance wire heat treatment and electromagnetic heating, and the addition ratio of the porous biochar material to the iron waste liquid is not higher than 100 g / L.

[0014] As preferred, in step c), in the initial stage of heating, electromagnetic heating and resistance wire heating act together, and after the temperature reaches the solidification load temperature or the resistance wire heating limit temperature, the resistance wire heating is turned off, and the remaining operation is completed using electromagnetic heating; the specified temperature is the resistance wire heating limit temperature or the solidification load temperature, the solidification load temperature is 400-800 DEG C, and the duration of the limited multi-heat source solidification load is 0.5-1 h.

[0015] As preferred, in step c), the special dispersed carrier is composed of a base, a "honeycomb briquette"-like isolator, and an end cover, the limitation is that the obtained adsorption material is only placed in each cylinder of the isolator, the effective space of a single limited cylinder of the special dispersed carrier is not higher than 110% of the volume of the adsorption material after uniform placement, and the special dispersed carrier is placed in the electromagnetic heating hollow metal block during the limited solidification load treatment.

[0016] As preferred, the surface of the iron source adsorption doped material contains nano iron oxide particles, and the iron load is not less than 1 wt.%.

[0017] The beneficial effects of the present application are:

[0018] 1. The present application can convert iron ions in industrial iron waste liquid into nano iron oxide particles and fix them in the structure of porous carbon material, realizing advanced utilization of waste metals, and through the use of ultrasonic and multi-heat source methods, energy consumption can be reduced, heating efficiency can be improved, and uniform heating can be achieved, and the compounds generated by activated biochar can also be reduced, not only solving the problem of industrial wastewater pollution, but also solving the problem of waste metal recycling, and at the same time realizing the energy storage application of the solidified material.

[0019] 2. The present application provides spatial sites for the adsorption of waste metal liquid ions through the pore structure of the porous biochar material, but since the adsorbed metal ions are mostly combined with the biochar by van der Waals force, electrostatic force, dispersion force or a small amount of chemical bond force, the thermal stability is poor, therefore, the present application adds a heat solidification treatment step to convert Fe into a stable functional group in the porous carbon.

[0020] 3. The present application can realize solidification-load integration, improve the stability and reusability of iron elements, and effectively avoid the loss of iron ions during solidification by subjecting the adsorption material to multi-heat source heat solidification treatment in a specially designed limited space.

[0021] 4. The application can utilize metal oxide particles to change the micro-pore structure, improve the electronic transmission capacity, electronic storage capacity and electronic transmission speed of carbon materials, thereby improving the energy density and specific capacitance, not only realizing the double waste utilization of waste marine products and industrial wastewater, but also expanding the application of biochar in energy storage technology, and having double significance for the development of energy storage technology and ecological environment protection.

[0022] The features and advantages of the present application will be described in detail with reference to the embodiments combined with the accompanying drawings.

DRAWINGS

[0023] Figure 1 is a process flow chart of a preparation method of the iron source adsorption doping material of the application;

[0024] Figure 2 is a special dispersion carrier placed in a tube furnace electromagnetic heating schematic diagram of the preparation method of the iron source adsorption doping material of the application;

[0025] Figure 3 is a special dispersion carrier structure schematic diagram of the preparation method of the iron source adsorption doping material of the application;

[0026] Figure 4 is the cyclic voltammetry test curve of the sample before and after adsorption of example one of the preparation method of the iron source adsorption doping material of the application;

[0027] Figure 5 is the constant current charge-discharge curve of the sample before and after adsorption of example two of the preparation method of the iron source adsorption doping material of the application.

[0028] Figure 6 is the constant current charge-discharge curve of the sample of example five of the preparation method of the iron source adsorption doping material of the application.

DETAILED DESCRIPTION

[0029] Example one:

[0030] The waste skin prawn is used as waste biomass, and the surface of the waste skin prawn is washed to remove impurities, and then dried. 10g of waste skin prawn is weighed and placed in a tube furnace at 600℃ under inert atmosphere for high temperature pyrolysis. After cooling, the biochar material is obtained. The specific surface area is measured to be 96m 2 / g;

[0031] a) 5g of biochar material is weighed and subjected to high-frequency ultrasonic modification treatment. The ultrasonic frequency is 100kHz, the ultrasonic time is 1.5h, and the ultrasonic temperature is 80℃;

[0032] b) 10 g / L of FeSO4 solution was configured to simulate industrial iron waste liquid, and then the biochar material after high-frequency ultrasonic modification treatment in step a) was added into the FeSO4 solution at an addition ratio of 5 g / L to perform low-frequency ultrasonic treatment, the ultrasonic frequency was 40 kHz, the ultrasonic interval was 15 minutes, the ultrasonic temperature was 25°C, and the adsorption time was 12 h;

[0033] c) The adsorption material after treatment in step b) was transferred to a special distributed carrier and placed in an inert atmosphere for single heat source curing heat treatment, and the finished product was obtained after cooling, wherein the heat curing treatment temperature was 550°C, the curing heat treatment time was 1 h, and the iron loading of the doped material was 1.6 wt.% through elemental analysis and x-ray photoelectron spectroscopy test analysis;

[0034] The iron source adsorption doped material prepared in step c), polytetrafluoroethylene and acetylene black were mixed in ethanol at a mass ratio of 7:2:1 to prepare a working electrode, and then the working electrode, platinum electrode and mercury electrode were combined to form a three-electrode test system, 4 mol / L Na2SO4 solution was used as electrolyte, and the cyclic voltammetry characteristics and constant current charge-discharge characteristics of the working electrode were tested by an electrochemical workstation. The specific capacitance of the electrode was 70 F / g at 1 A / g, and the specific capacitance of the undoped porous biochar was 77.7 F / g, with a performance improvement of 11%.

[0035] Example Two:

[0036] The waste skin of freshwater shrimp was used as waste biomass, and the surface was first washed to remove impurities and then dried. 10 g of waste skin of freshwater shrimp was weighed and pyrolyzed in a tube furnace at 600°C under an inert atmosphere. The biochar material was obtained after cooling, and the specific surface area was 95 m 2 / g;

[0037] a) 5 g of biochar material was subjected to high-frequency ultrasonic modification treatment, the ultrasonic frequency was 100 kHz, the ultrasonic time was 1.5 h, and the ultrasonic temperature was 80°C;

[0038] b) 10 g / L of FeSO4 solution was configured to simulate industrial iron waste liquid, and then the biochar material after high-frequency ultrasonic modification treatment in step a) was added into the FeSO4 solution at an addition ratio of 5 g / L to perform low-frequency ultrasonic treatment, 3% hydrogen peroxide was added 1 h before the end of the reaction, and a solenoid coil was used for magnetization treatment, the ultrasonic frequency was 40 kHz, the ultrasonic interval was 15 minutes, the ultrasonic temperature was 25°C, the adsorption time was 12 h, the concentration of the hydrogen peroxide was not less than 3%, and the solenoid coil was a solenoid magnetic field generating coil with a central magnetic field of 300 GS;

[0039] c) transferring the adsorbed material after step b) to a special designed dispersion carrier, and placing them together in an inert atmosphere for single heat source curing heat treatment, and the finished product is obtained after cooling, wherein the heat curing treatment temperature is 550℃, the curing heat treatment time is 1h, and the iron loading of the doped material is 2.9wt.% by elemental analysis and x-ray photoelectron spectroscopy test analysis;

[0040] The iron source adsorbed doped material prepared in step c), polytetrafluoroethylene and acetylene black are mixed in ethanol according to a mass ratio of 7:2:1 to prepare a working electrode, then the working electrode, a platinum electrode and a mercury-mercury electrode are combined to form a three-electrode test system, 4mol / L Na2SO4 solution is used as an electrolyte, and an electrochemical workstation is used to test the cyclic voltammetry characteristics and constant current charge-discharge characteristics of the working electrode, please refer to Figure 4 、 Figure 5 (a is the sample before adsorption, and b is the sample after adsorption), and the specific capacitance of the electrode at 0.8A / g is 95F / g, while the specific capacitance of the undoped porous biochar at 1A / g is 80F / g, and the performance is improved by 18.75%.

[0041] The biggest difference between Example Two and Example One is that the magnetization treatment is added during the low-frequency ultrasonic treatment, and the results show that the beneficial effect is improved.

[0042] Example Three:

[0043] The waste skin of freshwater shrimp is used as waste biomass, and the surface is first washed to remove impurities and then dried. 10g of waste skin of freshwater shrimp is weighed and pyrolyzed in a tube furnace at 600℃ under an inert atmosphere. After cooling, the biochar material is obtained, and the specific surface area is measured to be 94m 2 / g;

[0044] a) 5g of biochar material is weighed for high-frequency ultrasonic modification treatment, the ultrasonic frequency is 100kHz, the ultrasonic time is 1.5h, and the ultrasonic temperature is 80℃;

[0045] b) 100g / L of FeSO4 solution is configured to simulate industrial iron waste liquid, and 5g / L of biochar material after high-frequency ultrasonic modification treatment in step a) is added to the FeSO4 solution for low-frequency ultrasonic treatment. 3% hydrogen peroxide is added 1h before the reaction ends, and a solenoid coil is used for magnetization treatment, the ultrasonic frequency is 40kHz, the ultrasonic interval is 3 minutes every 15 minutes, the ultrasonic temperature is 25℃, the adsorption time is 12h, the concentration of the hydrogen peroxide is not less than 3%, and the solenoid coil is a solenoid magnetic field generating coil with a central magnetic field of 300GS;

[0046] c) the adsorbed material after step b) is filtered and transferred to a special distributed carrier, and then placed in an inert atmosphere for single heat source curing heat treatment, and the finished product is obtained after cooling, wherein the heat curing treatment temperature is 550℃, the curing heat treatment time is 1h, and the iron loading of the doped material is 5.4wt.% by elemental analysis and x-ray photoelectron spectroscopy test analysis;

[0047] The iron source adsorbed doped material prepared in step c), polytetrafluoroethylene and acetylene black are mixed in ethanol at a mass ratio of 7:2:1 to prepare a working electrode, then the working electrode, a platinum electrode and a mercury electrode are combined to form a three-electrode test system, 4mol / L Na2SO4 solution is used as an electrolyte, and an electrochemical workstation is used to test the cyclic voltammetry characteristics and constant current charge and discharge characteristics of the working electrode. The specific capacitance of the electrode is 107.7F / g at 1A / g, and the specific capacitance of the undoped porous biochar is 89F / g, and the performance is improved by 21%.

[0048] The biggest difference between example three and example two is that the concentration of adsorbed industrial wastewater is improved, and the results show that the beneficial effect is improved.

[0049] Example four:

[0050] The waste skin of freshwater shrimp is used as waste biomass, and the surface is first washed to remove impurities and then dried. 10g of waste skin of freshwater shrimp is placed in a tube furnace at 750℃ under an inert atmosphere for high temperature pyrolysis, and the biochar material is obtained after cooling. The specific surface area is 119m 2 / g;

[0051] a) 5g of biochar material is subjected to high-frequency ultrasonic modification treatment, the ultrasonic frequency is 100kHz, the ultrasonic time is 1.5h, and the ultrasonic temperature is 80℃;

[0052] b) 100g / L of FeSO4 solution is configured to simulate industrial iron waste liquid, and then 5g / L of biochar material after high-frequency ultrasonic modification treatment in step a) is added to the FeSO4 solution for low-frequency ultrasonic treatment. 3% hydrogen peroxide is added 1h before the reaction is completed, and a solenoid coil is used for magnetization treatment, the ultrasonic frequency is 40kHz, the ultrasonic interval is 3 minutes every 15 minutes, the ultrasonic temperature is 25℃, the adsorption time is 12h, the concentration of the hydrogen peroxide is not less than 3%, and the magnetization coil is a solenoid magnetic field generating coil with a central magnetic field of 300GS;

[0053] c) the adsorbed material after step b) is filtered and transferred to a special distributed carrier, and then placed in an inert atmosphere for single heat source curing heat treatment, and the finished product is obtained after cooling, wherein the heat curing treatment temperature is 750℃, the curing heat treatment time is 1h, and the iron loading of the doped material is 5.1wt.% by elemental analysis and x-ray photoelectron spectroscopy test analysis;

[0054] The iron source adsorbed doped material, polytetrafluoroethylene and acetylene black prepared in step c) are mixed in ethanol at a mass ratio of 7:2:1 to prepare a working electrode, then the working electrode is combined with a platinum electrode and a calomel electrode to form a three-electrode test system, 4 mol / L Na2SO4 solution is used as an electrolyte, and the cyclic voltammetry characteristics and constant current charge and discharge characteristics of the working electrode are tested by an electrochemical workstation. The specific capacitance of the electrode is 120.7 F / g at 1 A / g, and the specific capacitance of the undoped porous biochar is 96 F / g, and the performance is improved by 25.7%.

[0055] The biggest difference between example four and example three is that the curing heat treatment temperature is improved, and the results show that the beneficial effect is improved.

[0056] Example five:

[0057] The waste skin of freshwater shrimp is used as waste biomass. After washing the surface to remove impurities, drying, weighing 10g of waste skin of freshwater shrimp, and placing it in a tube furnace at 750℃ under inert atmosphere for high temperature pyrolysis, the biochar material is obtained after cooling. The specific surface area is 112m 2 / g;

[0058] a) 5g of biochar material is subjected to high-frequency ultrasonic modification treatment, the ultrasonic frequency is 100kHz, the ultrasonic time is 1.5h, and the ultrasonic temperature is 80℃;

[0059] b) 100g / L of FeSO4 solution is configured to simulate industrial iron waste liquid, and then 5g / L of biochar material after high-frequency ultrasonic modification treatment in step a) is added into the FeSO4 solution for low-frequency ultrasonic treatment. 3% hydrogen peroxide is added 1h before the reaction ends, and a solenoid coil is used for magnetization treatment. The ultrasonic frequency is 40kHz, the ultrasonic interval is 3 minutes every 15 minutes, the ultrasonic temperature is 25℃, the adsorption time is 12h, the concentration of the hydrogen peroxide is not less than 3%, and the solenoid coil is a solenoid magnetic field generating coil with a central magnetic field of 300GS;

[0060] c) The adsorbed material after step b) treatment is filtered and transferred to a specially designed distributed carrier, and is placed in an inert atmosphere for multi-heat source curing and loading. Initially, resistance wire heating and electromagnetic heating are used for cooperative heating. When the resistance wire heating reaches the limit temperature, the resistance wire heating is turned off, and the electromagnetic heating is used to complete the remaining operation. After cooling, the finished product is obtained. The heat curing treatment temperature is 750℃, and the curing heat treatment time is 1h. Element analysis and x-ray photoelectron spectroscopy test analysis show that the iron loading of the doped material is 5.6wt.%;

[0061] The iron source adsorbed doped material, polytetrafluoroethylene and acetylene black prepared in step c) are mixed in ethanol in a mass ratio of 7:2:1 to prepare a working electrode, then the working electrode is combined with a platinum electrode and a calomel electrode to form a three-electrode test system, 4 mol / L Na2SO4 solution is used as an electrolyte, and the cyclic voltammetry characteristics and constant current charge and discharge characteristics of the working electrode are tested by an electrochemical workstation, refer to Figure 6 , and the specific capacitance of the electrode is measured to be 131.3 F / g at 1 A / g.

[0062] The biggest difference between example five and example four is that multiple heat sources are used for heating during solidification and loading, and the results show that the beneficial effect is improved.

[0063] Example six:

[0064] The waste skin of freshwater shrimp is used as waste biomass. After washing and removing impurities, the waste skin of freshwater shrimp is dried. 10g of waste skin of freshwater shrimp is placed in a tube furnace at 750℃ under inert atmosphere for high temperature pyrolysis. After cooling, the biochar material is obtained. The specific surface area is measured to be 120m 2 / g;

[0065] a) 5g of biochar material is subjected to high-frequency ultrasonic modification treatment. The ultrasonic frequency is 100kHz, the ultrasonic time is 1.5h, and the ultrasonic temperature is 80℃;

[0066] b) 100g / L of FeSO4 solution is configured to simulate industrial iron waste liquid. 5g / L of biochar material modified by high-frequency ultrasonic in step a) is added to the FeSO4 solution for low-frequency ultrasonic treatment. 3% hydrogen peroxide is added 1h before the reaction ends, and a solenoid coil is used for magnetization treatment. The ultrasonic frequency is 40kHz, the ultrasonic interval is 3 minutes every 15 minutes, the ultrasonic temperature is 25℃, the adsorption time is 12h, the concentration of hydrogen peroxide is not less than 3%, and the solenoid coil is a solenoid magnetic field generating coil with a central magnetic field of 300GS;

[0067] c) The adsorbed material after step b) is filtered and transferred to a porcelain boat. A large porcelain boat is placed on a small porcelain boat, and both are placed in an inert atmosphere for multi-heat source solidification and loading. Initially, the resistance wire heating and electromagnetic heating are used for cooperative heating. When the resistance wire heating reaches the limit temperature, the resistance wire heating is turned off, and the electromagnetic heating is used to complete the remaining operation. After cooling, the finished product is obtained. The heat treatment temperature is 750℃, and the solidification heat treatment time is 1h. Element analysis and x-ray photoelectron spectroscopy test analysis show that the iron loading of the doped material is 5.5wt.%;

[0068] The iron source adsorbed doped material, polytetrafluoroethylene and acetylene black prepared in step c) are mixed in ethanol according to a mass ratio of 7:2:1 to prepare a working electrode, then the working electrode, a platinum electrode and a calomel electrode are combined to form a three-electrode test system, 4 mol / L Na2SO4 solution is used as an electrolyte, and an electrochemical workstation is used to test the cyclic voltammetry characteristics and constant current charge / discharge characteristics of the working electrode, and it is found that the specific capacitance of the electrode is 116.8 F / g at 1 A / g, and the specific capacitance of the undoped porous biochar is 91 F / g, and the performance is improved by 28.3%.

[0069] The biggest difference between example six and example five is that the special distributed carrier is used in the confinement of example five, and the results show that the beneficial effect is improved.

[0070] The above examples are descriptions of the application, not limitations of the application, and any simple transformation of the application also belongs to the protection scope of the application.

Claims

1. A method for preparing an iron source adsorption doped material, characterized in that, Includes the following steps: a) High-frequency ultrasonic modification: Biochar material prepared from waste biomass after pyrolysis is subjected to high-frequency ultrasonic modification treatment. The ultrasonic frequency of the high-frequency ultrasonic modification is 80~200kHz, the high-frequency ultrasonic time is 1~3h, and the high-frequency ultrasonic temperature is 70~100℃. After filtration, ultrasonically modified biochar material is obtained. Using the ultrasonically modified biochar material as a substrate and industrial iron waste liquid as an iron source, the ultrasonically modified biochar material and industrial iron waste liquid are mixed to obtain a solid-liquid mixture. b) Low-frequency ultrasonic magnetization treatment: The solid-liquid mixture prepared in step a) is subjected to intermittent low-frequency ultrasonic oscillation adsorption, then hydrogen peroxide solution is added and an electromagnetic coil is passed through. After reacting for 0.5~1h, it is filtered, and then washed multiple times to remove the waste metal liquid and dried to obtain the adsorbent material. The ultrasonic frequency of the low-frequency ultrasonic magnetization treatment is 30~60kHz, the low-frequency ultrasonic interval is 3 minutes every 15 minutes, the low-frequency ultrasonic temperature is 20~40℃, the adsorption time is 12~48h, the concentration of hydrogen peroxide is not less than 3%, and the magnetization coil is a solenoid magnetic field generating coil with a central magnetic field of not less than 300GS. c) Confined Multi-Heat Source Curing Load: The adsorbent material prepared in step b) is uniformly placed in a specially designed dispersion carrier and subjected to resistance wire-electromagnetic multi-heat source curing load treatment. The specially designed dispersion carrier consists of a base, a "honeycomb"-shaped isolator, and end caps. The confinement specifically means that the obtained adsorbent material is placed only in each cylinder of the isolator. The effective space of a single confined cylinder of the specially designed dispersion carrier is no more than 110% of the volume of the adsorbent material after uniform placement. During the confined curing load treatment, the specially designed dispersion carrier is placed in an electromagnetically heated hollow metal block. At the beginning of heating, resistance wire heating and electromagnetic heating work together. After reaching the specified temperature for 5 minutes, the resistance wire heating is turned off. The curing load temperature is maintained for a period of time, and then the product is cooled to obtain the finished product. The specified temperature is the resistance wire heating limit temperature or the curing load temperature. The curing load temperature is 400~800℃, and the confined multi-heat source curing load time is 0.5~1h.

2. The method for preparing an iron source adsorption doped material as described in claim 1, characterized in that: In step a), the iron ion concentration of the industrial iron waste liquid is not less than 0.1 g / L.

3. The method for preparing an iron source adsorption doped material as described in claim 2, characterized in that: The industrial iron waste liquid includes organic liquid phase pollutants containing ferrous ions, organic liquid phase pollutants containing ferric ions, and inorganic liquid phase pollutants containing ferric ions.

4. The method for preparing an iron source adsorption doped material as described in claim 1, characterized in that: In step c), the heating method for the multi-heat source curing load is a combination of resistance wire heat treatment and electromagnetic heating; in step a), the addition ratio of the ultrasonically modified biochar material to the iron waste liquid is not higher than 100 g / L.

5. The method for preparing an iron source adsorption doped material as described in claim 1, characterized in that: The surface of the iron source adsorption doping material contains nano-iron oxide particles, and the iron loading in the iron source adsorption doping material is not less than 1 wt.%.

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