CN110759711A - Method for preparing spherical ceramic composite microwave absorbing material by utilizing coal gangue - Google Patents
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Abstract
The invention provides a method for preparing a spherical ceramic composite microwave absorbing material by utilizing coal gangue, belonging to the technical field of microwave absorbing materials. The technical scheme is as follows: firstly, ball milling and screening coal gangue to obtain coal gangue powder, slowly spraying a binder and a metal salt ion solution for granulation to form coal gangue-based composite microspheres, and then drying and carrying out in-situ carbothermic reduction on the composite microspheres to obtain the composite microwave absorbing material loaded with series magnetic components. The method takes the solid waste coal gangue as the raw material, realizes the effective recycling of the coal gangue, and saves resources and cost; meanwhile, the in-situ granulation-loading process can ensure that the loading substance is uniformly dispersed on the coal gangue particle carrier, has simple and convenient operation process and easy implementation, and is suitable for large-scale industrial production application.
Description
Technical Field
The invention belongs to the technical field of microwave absorbing material preparation processes, and particularly relates to a method for preparing a spherical ceramic composite microwave absorbing material by utilizing coal gangue.
Background
With the rapid development of modern electronic information technology, more and more electronic devices become important tools essential for our lives and works, and are widely applied to the military field (radar) and the civil field (computer, navigation, communication and electrical equipment), thereby making great contribution to the progress and development of society. At the same time, people are also faced with the increasingly serious problem of electronic equipment radiation. In the modern society, electromagnetic wave radiation is a new pollution source following water pollution, air pollution and noise pollution, and not only can interfere communication, but also seriously harms human health.
The coal gangue is an industrial solid waste, is produced in the coal mining, washing and processing processes and accounts for 10 to 25 percent of the total amount of the coal. In China, the annual emission amount of coal gangue is about 2.8 hundred million tons, and the coal gangue becomes one of the largest solid wastes in emission and accumulation. Meanwhile, improper storage and disposal of coal gangue can cause serious environmental pollution to surrounding soil and groundwater and pose serious threats to human health and ecosystem. Therefore, recycling these wastes has been a challenge for geotechnical and environmental engineers. However, coal gangue is an available resource, and can replace fuel to generate electricity to produce chemical products such as aluminum chloride, water glass and the like. However, the coal gangue utilization in this way has not been promoted because of high production cost and low profit. At present, the coal gangue is mainly used for power generation, agricultural fertilizer, highway subgrade, brick production, cement production and concrete production. Therefore, finding a suitable coal gangue utilization method has become a focus of research.
In view of the above, if the coal gangue can be recycled to prepare the microwave absorbing material, not only the pollution caused by the discharge and accumulation of the coal gangue can be eliminated, but also the economic benefit and the social benefit are significant, and more importantly, a new idea is provided for the comprehensive utilization of the solid waste.
Disclosure of Invention
In order to overcome the defects in the prior art, solve the pollution problem caused by the discharge and accumulation of coal gangue and achieve the effect of treating pollution by waste, the coal gangue is recycled to prepare the microwave absorbing material, and the invention provides a method for preparing the spherical ceramic composite microwave absorbing material by utilizing the coal gangue.
The invention is realized by the following technical scheme:
a method for preparing a spherical ceramic composite microwave absorbing material by utilizing coal gangue comprises the following steps:
s1, ball-milling the coal gangue, screening by a 100-300-mesh standard sieve, drying the screened coal gangue powder for 3-4 hours at 80-100 ℃, and reserving the dried coal gangue powder for later use;
s2, preparing solution A: preparing a sodium carboxymethylcellulose aqueous solution with the concentration of 0.1-6 wt% as a solution A for later use;
s3, preparing a solution B: preparing a salt solution with the concentration of 0.5-2 mol/L as a B solution for later use; the solution B contains Fe3+、Co2+、Ni2+Or a salt solution of one or both of them, or containing Fe3+–Mn2+A salt solution;
s4, placing the gangue powder prepared in the step S1 in an Aili powerful mixer, slowly spraying the solution A prepared in the step S2 and the solution B prepared in the step S3 into the mixer to start granulation and balling, and preparing the gangue-based composite microspheres, wherein the ratio of the gangue powder to the solution A to the solution B is 15 g: 1mL of: 1.5-3 mL;
a granulating and balling process features that the sprayed water drops adsorb the coal gangue micropowder to form small balls, which are then stirred by mixer to make circular and reciprocating movement while more coal gangue micropowder grows up, and the sprayed water drops are adhered to the surface of balls for cyclic granulating. In the operation, the metal inorganic salt ion solution is sprayed, so that the metal ions can be uniformly distributed in the coal gangue base material ball and on the surface of the coal gangue base material ball, and the caking agent sodium carboxymethyl cellulose solution with certain concentration is added in the ball forming process in an auxiliary way due to poor plasticity of the coal gangue, thereby improving the ball forming efficiency and quality;
s5, placing the gangue-based composite microspheres prepared in the step S4 in an oven, drying for 12 hours at 30-50 ℃, sintering at the constant temperature of 400-900 ℃ for 2-3 hours in an inert gas atmosphere, and cooling to room temperature along with the oven to prepare the spherical ceramic composite microwave absorbing material;
the gangue-based microspheres obtained after drying are subjected to reduction treatment in an inert atmosphere to obtain the composite material loaded with different magnetic components, and the magnetic components are generated on gangue particles by in-situ carbothermic reduction reaction of fixed carbon components (about 20 wt%) in the gangue components, so that the obtained composite wave-absorbing material is uniform in composition and structure. In addition, part of the remaining fixed carbon still remains after high-temperature treatment, the graphitization degree of the carbon is also improved under the catalytic action of the magnetic component, the dielectric loss of the composite material is favorably enhanced, and the material is finally ensured to have good wave-absorbing performance.
Furthermore, the prepared spherical composite microwave absorbing material has magnetism, and the magnetic components comprise simple substance Fe, simple substance Co, simple substance Ni and Fe3O4、CoFe2O4、NiFe2O4、NiCo2O4、MnFe2O4、One or more of FeCo alloy, FeNi alloy, CoNi alloy and FeMn alloy.
Compared with the prior art, the invention has the beneficial effects that:
(1) the in-situ granulation-loading process used by the invention realizes that the loading materials are uniformly dispersed on the coal gangue-based microspheres, and compared with the traditional chemical synthesis process comprising a precipitation method, a hydrothermal method, chemical plating and a chemical vapor deposition method, the method is simpler and the loading effect of the magnetic components is better.
(2) The raw material coal gangue used by the invention is solid waste, has wide source and low cost, and is suitable for large-scale popularization and application.
(3) The coal gangue is not subjected to separation, purification and modification treatment, is directly used after being crushed, is not limited by regions and production places, and really realizes high-efficiency recycling of the coal gangue.
(4) Although the coal gangue is solid waste, the coal gangue still contains about 20wt% of fixed carbon, the coal gangue is skillfully utilized, and in the inert atmosphere sintering process (400-900 ℃) after granulation, balling and drying processes, the part of fixed carbon plays a role of a reducing agent, and a magnetic component precursor loaded on the coal gangue microspheres can be gradually reduced to generate corresponding magnetic oxides, metal simple substances or alloys.
Drawings
Fig. 1 is a microwave absorption curve of the wave-absorbing material prepared in example 2 at different coating thicknesses.
FIG. 2 is an X-ray diffraction pattern of the wave-absorbing material prepared in example 3.
Detailed Description
To explain technical solutions, structural features, and technical effects of the present invention in detail, the following detailed description is given with reference to the accompanying drawings in conjunction with the detailed description. The following examples are merely illustrative of the present invention and should not be construed as limiting the scope of the invention.
Example 1
A method for preparing a spherical ceramic composite microwave absorbing material by utilizing coal gangue comprises the following steps:
s1, ball-milling the coal gangue, screening by a 300-mesh standard sieve, drying the screened coal gangue powder for 3.5 hours at 90 ℃, and reserving the dried coal gangue powder for later use;
s2, preparing solution A: preparing 1wt% sodium carboxymethylcellulose aqueous solution as solution A for later use;
s3, preparing solution B: fe is contained at a concentration of 1.25mol/L3+–Ni2+Salt solution is used as B solution;
s4, placing the gangue powder prepared in the step S1 in an Aili powerful mixer, slowly spraying the solution A prepared in the step S2 and the solution B prepared in the step S3 into the mixer to start granulation and balling, and preparing the gangue-based composite microspheres, wherein the ratio of the gangue powder to the solution A to the solution B is 15 g: 1mL of: 2.5 mL;
s5, placing the gangue-based composite microspheres prepared in the step S4 in an oven, drying for 12 hours at 40 ℃, sintering for 3 hours at the constant temperature of 800 ℃ in an inert gas atmosphere, and cooling to room temperature along with the oven to prepare the spherical FeNi alloy-loaded ceramic composite microwave absorbing material.
Example 2
A method for preparing a spherical ceramic composite microwave absorbing material by utilizing coal gangue comprises the following steps:
s1, ball-milling the coal gangue, screening by a 200-mesh standard sieve, drying the screened coal gangue powder for 3 hours at 100 ℃, and reserving the dried coal gangue powder for later use;
s2, preparing solution A: preparing a sodium carboxymethylcellulose aqueous solution with the concentration of 2wt% as a solution A for later use;
s3, preparing a solution B: fe is contained at a concentration of 1.5 mol/L3+Salt solution is used as B solution;
s4, placing the gangue powder prepared in the step S1 in an Aili powerful mixer, slowly spraying the solution A prepared in the step S2 and the solution B prepared in the step S3 into the mixer to start granulation and balling, and preparing the gangue-based composite microspheres, wherein the ratio of the gangue powder to the solution A to the solution B is 15 g: 1mL of: 3 mL;
s5, drying the coal gangue-based composite microspheres prepared in the step S4 in an oven at 40 ℃ for 12 hours, sintering at 600 ℃ for 2 hours under an inert gas atmosphere, and cooling to room temperature along with the oven to obtain spherical load Fe and Fe3O4The ceramic composite microwave absorbing material.
As can be seen from FIG. 1, on the reflection loss curve (2-18 GHz) of the ceramic composite wave-absorbing material prepared in example 2, the lowest reflection loss values of the frequency in the range of 3-18 GHz are all lower than-10 dB along with the change of the coating thickness (1.5-5.5 mm) of the wave-absorbing material.
Example 3
A method for preparing a spherical ceramic composite microwave absorbing material by utilizing coal gangue comprises the following steps:
s1, ball-milling the coal gangue, screening by a 150-mesh standard sieve, drying the screened coal gangue powder for 4 hours at 80 ℃, and reserving the dried coal gangue powder for later use;
s2, preparing solution A: preparing a sodium carboxymethylcellulose aqueous solution with the concentration of 5wt% as a solution A for later use;
s3, preparing a solution B: co-containing solution with a concentration of 2mol/L2+Salt solution is used as B solution;
s4, placing the gangue powder prepared in the step S1 in an Aili powerful mixer, slowly spraying the solution A prepared in the step S2 and the solution B prepared in the step S3 into the mixer to start granulation and balling, and preparing the gangue-based composite microspheres, wherein the ratio of the gangue powder to the solution A to the solution B is 15 g: 1mL of: 3 mL;
s5, drying the gangue-based composite microspheres prepared in the step S4 in an oven at 40 ℃ for 12 hours, sintering at the constant temperature of 800 ℃ for 3 hours in an inert gas atmosphere, and cooling to room temperature along with the oven to obtain the spherical simple substance Co-loaded ceramic composite microwave absorbing material.
As can be seen from FIG. 2, the phase composition of the supported material obtained in example 3 is simple Co, which indicates that Co can be contained in the supported material by carbothermic reduction treatment at 800 ℃ for 3 hours2+The precursor is reduced to obtain a Co simple substance, and the rest diffraction peaks in the map correspond to phases of the carrier.
Example 4
A method for preparing a spherical ceramic composite microwave absorbing material by utilizing coal gangue comprises the following steps:
s1, ball-milling the coal gangue, screening by a 240-mesh standard sieve, drying the screened coal gangue powder for 3 hours at 100 ℃, and reserving the dried coal gangue powder for later use;
s2, preparing solution A: preparing a sodium carboxymethylcellulose aqueous solution with the concentration of 3wt% as a solution A for later use;
s3, preparing a solution B: fe is contained at a concentration of 1.25mol/L3+–Mn2+Salt solution is used as B solution;
s4, placing the gangue powder prepared in the step S1 in an Aili powerful mixer, slowly spraying the solution A prepared in the step S2 and the solution B prepared in the step S3 into the mixer to start granulation and balling, and preparing the gangue-based composite microspheres, wherein the ratio of the gangue powder to the solution A to the solution B is 15 g: 1mL of: 2 mL;
s5, placing the gangue-based composite microspheres prepared in the step S4 in an oven, drying for 12 hours at 50 ℃, sintering for 3 hours at the constant temperature of 900 ℃ in an inert gas atmosphere, and cooling to room temperature along with the oven to prepare the spherical FeMn alloy-loaded ceramic composite microwave absorbing material.
Example 5
A method for preparing a spherical ceramic composite microwave absorbing material by utilizing coal gangue comprises the following steps:
s1, ball-milling the coal gangue, screening by a 200-mesh standard sieve, drying the screened coal gangue powder for 3 hours at 100 ℃, and reserving the dried coal gangue powder for later use;
s2, preparing solution A: preparing a sodium carboxymethylcellulose aqueous solution with the concentration of 3wt% as a solution A for later use;
s3, preparing a solution B: fe-containing solution with the concentration of 1mol/L3+–Co2+Salt solution is used as B solution;
s4, placing the gangue powder prepared in the step S1 in an Aili powerful mixer, slowly spraying the solution A prepared in the step S2 and the solution B prepared in the step S3 into the mixer to start granulation and balling, and preparing the gangue-based composite microspheres, wherein the ratio of the gangue powder to the solution A to the solution B is 15 g: 1mL of: 3 mL;
s5, placing the coal gangue-based composite microspheres prepared in the step S4 into an ovenDrying at 50 deg.C for 12 hr, sintering at 600 deg.C under inert gas atmosphere for 2 hr, and cooling to room temperature to obtain spherical FeCo and CoFe loaded2O4The ceramic composite microwave absorbing material.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed, and any modifications or alterations which may be readily apparent to those skilled in the art are intended to be within the scope of the invention as defined by the appended claims. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (2)
1. A method for preparing a spherical ceramic composite microwave absorbing material by utilizing coal gangue is characterized by comprising the following steps:
s1, ball-milling the coal gangue, screening by a 100-300-mesh standard sieve, drying the screened coal gangue powder for 3-4 hours at 80-100 ℃, and reserving the dried coal gangue powder for later use;
s2, preparing solution A: preparing a sodium carboxymethylcellulose aqueous solution with the concentration of 0.1-6 wt% as a solution A for later use;
s3, preparing a solution B: preparing a salt solution with the concentration of 0.5-2 mol/L as a B solution for later use; the solution B contains Fe3+、Co2+、Ni2+Or a salt solution of one or both of them, or containing Fe3+–Mn2+A salt solution;
s4, placing the gangue powder prepared in the step S1 in an Aili powerful mixer, slowly spraying the solution A prepared in the step S2 and the solution B prepared in the step S3 into the mixer to start granulation and balling, and preparing the gangue-based composite microspheres, wherein the ratio of the gangue powder to the solution A to the solution B is 15 g: 1mL of: 1.5-3 mL;
and S5, drying the gangue-based composite microspheres prepared in the step S4 in an oven at 30-50 ℃ for 12 hours, sintering at 400-900 ℃ for 2-3 hours under an inert gas atmosphere, and cooling to room temperature along with the oven to obtain the spherical ceramic composite microwave absorbing material.
2. The method for preparing the spherical ceramic composite microwave absorbing material by using the coal gangue as claimed in claim 1, wherein the method comprises the following steps: the prepared spherical composite microwave absorbing material has magnetism, and the magnetic components comprise simple substance Fe, simple substance Co, simple substance Ni and Fe3O4、CoFe2O4、NiFe2O4、NiCo2O4、MnFe2O4、One or more of FeCo alloy, FeNi alloy, CoNi alloy and FeMn alloy.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112441815A (en) * | 2020-12-04 | 2021-03-05 | 太原科技大学 | Method for preparing microwave absorbing material by utilizing red mud and coal gangue and application thereof |
| CN113860905A (en) * | 2021-10-27 | 2021-12-31 | 太原科技大学 | Method for preparing ceramic composite microwave absorbing material by utilizing red mud |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108610015A (en) * | 2018-06-08 | 2018-10-02 | 太原科技大学 | A kind of microwave absorbing material preparation method based on gangue |
| CN108675765A (en) * | 2018-06-08 | 2018-10-19 | 太原科技大学 | A kind of microwave absorbing material preparation method based on gangue |
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| CN112441815A (en) * | 2020-12-04 | 2021-03-05 | 太原科技大学 | Method for preparing microwave absorbing material by utilizing red mud and coal gangue and application thereof |
| CN113860905A (en) * | 2021-10-27 | 2021-12-31 | 太原科技大学 | Method for preparing ceramic composite microwave absorbing material by utilizing red mud |
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