CN110127690B - Method for preparing expanded graphite by adopting continuous detonation pressure release technology - Google Patents
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Abstract
The invention provides a method for preparing expanded graphite by adopting a continuous detonation pressure release technology, belonging to the field of material preparation. The method comprises the following steps: (1) mixing materials: adding graphite powder into a proper amount of polar solvent to form a solid-liquid mixture, and uniformly stirring; (2) granulation: adding the material obtained in the step (1) into a bonding agent, stirring into slurry, and preparing into spherical particles with the diameter of 1 cm; (3) drying: drying the material obtained in the step (2) to the moisture content of 1-5%; (4) continuous detonation: putting the material obtained in the step (3) into a closed container, introducing saturated steam to increase the pressure to 0.5-2.5MP, maintaining the pressure for 50-180s, and releasing the pressure to the atmospheric pressure within 87 milliseconds; continuously carrying out detonation and detonation pressure release treatment on the material for multiple times; (5) separating and drying: and (5) separating and drying the material obtained in the step (4) to obtain the expanded graphite. The invention does not need to add strong oxidant, thus avoiding the pollution to the environment; easy operation and suitability for industrial production.
Description
Technical Field
The invention belongs to the field of material preparation, and particularly relates to a method for preparing expanded graphite by adopting a continuous detonation pressure release technology.
Background
Expanded Graphite (EG) is a loose, porous, vermicular novel carbon material prepared from Graphite serving as a raw material. Inserting some substances into graphite layers by a chemical or physical method to form expandable graphite, then carrying out instantaneous high-temperature treatment, and increasing the interlayer spacing of the graphite along the C-axis direction when the pressure generated between the expandable graphite layers is greater than the Van der Waals force between the graphite layers to form the expandable graphite. The expanded graphite has the advantages of light weight, large specific surface area, adsorption with nonpolar molecular adsorption property, excellent electric and heat conduction properties and the like on a macroscopic scale, and therefore, the expanded graphite is widely applied to the fields of sealing materials, adsorption materials, electrode materials and the like.
At present, methods for preparing expanded graphite generally include a high temperature method, a laser method, a microwave method, an explosion method, and the like, and among them, the most widely used method is the high temperature method; chinese patent CN105502360B discloses a method for preparing sulfur-free expandable graphite, which takes crystalline flake graphite as a raw material and potassium permanganate and perchloric acid as intercalation agents, and the expanded graphite is prepared by expansion in a high-temperature muffle furnace. However, the high temperature method for preparing the expanded graphite often requires a strong oxidant, such as potassium permanganate, sulfuric acid, etc., which increases the risk and causes environmental pollution. Therefore, the method for preparing the expanded graphite by adopting the continuous detonation pressure release technology is provided, and the potassium permanganate, the sulfuric acid and other strong oxidants are not required to be added in the preparation process, so that the pollution to the environment is avoided; the detonation pressure release treatment is safe and energy-saving, the operation is simple, and the large-scale preparation is facilitated.
Disclosure of Invention
The invention aims to provide a simple and environment-friendly method for preparing expanded graphite, and particularly relates to a method for preparing expanded graphite by adopting a continuous detonation pressure release technology.
The technical scheme of the invention is as follows: a method for preparing expanded graphite by adopting a continuous detonation pressure release technology is characterized by comprising the following steps:
(1) Mixing materials: adding graphite powder into a proper amount of polar solvent to form a solid-liquid mixture, and uniformly stirring;
(2) And (3) granulation: adding a proper amount of adhesive into the material obtained in the step (1), and uniformly stirring the mixture into slurry to prepare spherical particles with the diameter of 1 cm;
(3) And (3) drying: drying the material obtained in the step (2) until the moisture content is 1-5%;
(4) Continuous detonation: putting the material obtained in the step (3) into a closed container for detonation pressure release treatment, namely introducing saturated steam into the container to increase the pressure to 0.5-2.5MP, keeping the pressure for 50-180s, and releasing the pressure to the atmospheric pressure by a mode of opening an end cover of the closed container in a flash manner within 87.5 milliseconds; continuously carrying out detonation and detonation pressure release treatment on the material for multiple times;
(5) Separation and drying: and (4) separating and drying the material obtained in the step (4) to obtain the expanded graphite.
The detonation pressure release technology adopted by the invention is that high-pressure steam is introduced into a closed container in which a material to be treated is stored, the high-temperature and high-pressure state is maintained for a certain time after the pressure reaches a set pressure, then the closed container is opened by instant ejection within 87.5 milliseconds, the pressure is released to normal pressure instantly (the pressure is released by ejection after the material is maintained for 4-10 minutes at 1-3MP, researches show that the air pressure balance time between the inside and the outside of a material microporous structure is about 1 second), and the material and the water vapor are exploded and discharged. Because the action time is extremely short, the energy density is extremely high, and the concentrated action is carried out in the material, the water vapor molecules and the internal combined water which permeate into the material and are among the molecules are released at a high speed in an extremely short time under the action of a strong vapor pressure difference, the potential energy accumulated by the pressure difference is converted into the kinetic energy for expansion work, and the water vapor molecules and the material are strongly impacted, thereby having obvious influence on the treatment process of the material.
The processing process of the detonation pressure release technology is divided into a high-temperature high-pressure maintaining stage and a pressure release stage. The hydrothermal chemical reaction takes place in a high-temperature high-pressure stage. In the pressure releasing stage, because the pressure releasing process time is millisecond grade, the inside of the closed container can hardly exchange heat with the outside, so that the instant pressure releasing process of the material and the water vapor becomes an adiabatic expansion heat power conversion process, and most of heat energy is converted into impact kinetic energy of gas and the material.
Although the existing 'steam explosion' technology also has a high-temperature high-pressure process and a rapid explosion process, the existing steam explosion technology cannot achieve the degree of adiabatic expansion work in the invention because the understanding of the thermodynamic principle of explosion pressure release is not in place, and the fastest pressure release moment is limited by the existing pressure release device and the principle to be less than 0.5 second which is far more than 87.5 milliseconds in the invention. The data are obtained by thermodynamic calculation analysis.
FIG. 1 is an X-ray diffraction (XRD) pattern of graphite and the expanded graphite prepared in example 1 wherein (a) is graphite; and (b) is expanded graphite. As can be seen from fig. 1, in the method for preparing expanded graphite by using the continuous detonation pressure releasing technology, the graphite and the prepared expanded graphite respectively have obvious diffraction peaks at 2 θ =26.55 ° and 2 θ =26.18 °, and the lattice spacing d =0.335nm of the graphite can be obtained by calculation according to the bragg equation, and the lattice spacing of the prepared expanded graphite is enlarged to d =0.340nm, which indicates that the interlayer spacing of the graphite is effectively enlarged by the detonation pressure releasing treatment; the average thickness of graphite crystal grains perpendicular to the crystal plane direction is D =53.12nm calculated according to the Scherrer formula, the average thickness of the prepared expanded graphite is about D =51.38nm, meanwhile, the full width at half maximum of a diffraction peak is increased, and the intensity of the diffraction peak is obviously reduced, which shows that the crystallinity of the prepared expanded graphite is reduced, the degree of structural order of the graphite is reduced, and the formation of the expanded graphite is confirmed.
The invention adopts the polar solvent to dissolve the binder, has good dispersion effect, ensures that the binder and the material are fully and uniformly mixed by stirring, is easy to prepare graphite powder into uniform spherical particles, and creates conditions for recovering the material after subsequent continuous multiple detonation pressure release treatment. Through exploration, the technical parameters of continuous and repeated detonation pressure release treatment are that the pressure in the tank is 0.5-2.5MP, the pressure maintaining time is 50-180s, and the pressure is released to the atmospheric pressure by a mode of opening an end cover of the closed container in a flash way within 87 milliseconds, so that the specific detonation pressure release treatment is completed. Each of these characteristic detonation pressure relief treatments results in a certain increase in the inter-laminar spacing of the graphite.
Microscopically, the distance between the inner graphite sheets is gradually increased along with the increase of the detonation treatment times; macroscopically, the expansion degree of the graphite after detonation pressure release treatment is higher and higher, and the expanded graphite is obtained through continuous multiple treatments.
The technical scheme of the invention has the following optimization or/and improvement:
one of the preferable technical schemes is as follows: the polar solvent in the step (1) comprises water, alcohol or a mixture thereof;
the second preferred technical scheme is as follows: the binder in the step (2) comprises one of emulsifier OP-10, carboxymethyl cellulose, polyvinyl alcohol emulsion, polytetrafluoroethylene emulsion, silicon rubber and the like;
the third preferred technical scheme is as follows: the material drying mode in the step (3) is to put the material into a drying box, heat the material to 30-60 ℃ and dry the material for 30-60min;
the fourth preferred technical scheme is as follows: the continuous detonation frequency in the step (4) is 50-500.
The expanded graphite prepared by the method has the beneficial effects that:
1. the special detonation pressure release treatment technology adopted by the invention can release pressure to atmospheric pressure within 87.5 milliseconds, a strong oxidant is not required to be added in the preparation process, the safety coefficient is improved, no harmful substance is generated in the preparation process, and the method is environment-friendly;
2. the graphite powder is made into spherical particles, and the spherical particles have a structure similar to honeycomb briquette, and the small granular graphite spheres can bear multiple times of detonation and detonation pressure release treatment under high pressure, so that the produced materials can be recovered. The powdery material cannot be recovered after detonation pressure release treatment;
3. the method has the advantages of simple operation and low energy consumption, is beneficial to large-scale preparation, and realizes industrial production.
The invention is further illustrated with reference to figure 1 and the specific examples.
Drawings
Fig. 1 is an X-ray diffraction (XRD) pattern of graphite and expanded graphite prepared in example 1, wherein (a) is graphite in fig. 1; and (b) the expanded graphite prepared in example 1.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to fig. 1 and specific examples.
Example 1
(1) Mixing materials: adding 20g of graphite powder into 20ml of ethanol solution (with the mass concentration of 99.7%) to form a solid-liquid mixture, and uniformly stirring;
(2) And (3) granulation: adding 0.2g of polyvinyl alcohol emulsion (with the mass concentration of 5%) into the material obtained in the step (1), uniformly stirring the mixture into slurry, and preparing spherical particles with the diameter of 1cm, namely the micro honeycomb briquette-shaped small graphite spheres;
(3) And (3) drying: putting the material obtained in the step (2) into an electrothermal constant-temperature drying oven at 30 ℃ for drying for 30min until the water content is 1.6%;
(4) Continuous detonation: putting the material obtained in the step (3) into a closed container for detonation pressure release treatment, namely introducing saturated steam into the container to increase the pressure to 2MP, keeping the pressure for 60s, and releasing the pressure to the atmospheric pressure within 87.5 milliseconds; continuously carrying out 50 times of detonation pressure release treatment on the material to obtain a black product in a reaction bin;
(5) Separation and drying: and (4) separating and drying the material obtained in the step (4) to obtain the expanded graphite.
As shown in fig. 1, the graphite and the prepared expanded graphite respectively have obvious diffraction peaks at 2 θ =26.55 ° and 2 θ =26.18 °, and the lattice spacing d =0.335nm of the graphite can be calculated according to the bragg equation, and the lattice spacing of the prepared expanded graphite is enlarged to d =0.340nm, which indicates that the interlayer spacing of the graphite is effectively enlarged by the detonation-detonation pressure-release treatment; the average thickness of the graphite crystal grain perpendicular to the crystal plane direction is calculated according to the Scherrer formula and is D =53.12nm, the average thickness of the prepared expanded graphite is about D =51.38nm, meanwhile, the full width at half maximum of a diffraction peak is increased, the intensity of the diffraction peak is obviously reduced, the crystallinity of the prepared expanded graphite is reduced, the degree of order of the graphite structure is reduced, and the formation of the expanded graphite is confirmed.
Table 1 shows the variation of the diffraction peak angle (2 θ), the lattice spacing (D) and the average thickness (D) of crystal grains of the samples perpendicular to the crystal plane for each example.
The bragg equation is: 2dsin θ = n λ
In the formula: d-diffraction lattice spacing; theta-diffraction angle; n-order of diffraction; lambda-the incident wavelength.
The Scherrer formula is: d = K λ/Bcos θ
In the formula: d-average thickness (nm) of crystal grains perpendicular to the crystal plane direction; K-Scherrer constant K =0.89; b-actually measuring the diffraction full width at half maximum of the sample; theta-diffraction angle; λ -X-ray wavelength, λ =0.154056nm.
Example 2
(1) Mixing materials: adding 20g of graphite powder into 20ml of ethanol solution (with the mass concentration of 99.7 percent), and uniformly stirring;
(2) And (3) granulation: adding 0.2g of polytetrafluoroethylene emulsion (with the mass concentration of 5%) into the material obtained in the step (1) as an adhesive, and uniformly stirring the mixture into slurry to prepare spherical particles with the diameter of 1cm, namely the micro honeycomb coal-shaped graphite spheres;
(3) And (3) drying: putting the material obtained in the step (2) into an electrothermal constant-temperature drying oven at 30 ℃ for drying for 50min until the water content is 1.2%;
(4) Continuous detonation: putting the material obtained in the step (3) into a closed container for detonation pressure release treatment, namely introducing saturated steam into the container to increase the pressure to 1.5MP, keeping the pressure for 90s, and releasing the pressure to the atmospheric pressure within 87.5 milliseconds; continuously carrying out detonation and detonation pressure release treatment on the material for 100 times; obtaining a black product in the reaction bin;
(5) Separation and drying: and (4) separating and drying the material obtained in the step (4) to obtain the expanded graphite.
The expanded graphite prepared in the embodiment has a remarkable diffraction peak at 2 theta =26.11 degrees, the lattice spacing is expanded to D =0.341nm, and the average thickness of the expanded graphite D =52.41nm.
Example 3
(1) Mixing materials: adding 20g of graphite powder into 20ml of ethanol solution (with the mass concentration of 50%), and uniformly stirring;
(2) And (3) granulation: adding 0.5g of emulsifier OP-10 (the mass concentration is 5%) into the material obtained in the step (1) as a bonding agent, uniformly stirring the mixture into slurry, and preparing spherical particles with the diameter of 1cm, namely the micro honeycomb coal-shaped graphite spheres;
(3) And (3) drying: putting the material obtained in the step (2) into an electrothermal constant-temperature drying oven at 60 ℃ for drying for 30min until the water content is 1.8%;
(4) Continuous detonation: putting the material obtained in the step (3) into a closed container for detonation pressure release treatment, namely introducing saturated steam into the container to increase the pressure to 2MP, keeping the pressure for 60s, and releasing the pressure to the atmospheric pressure within 87.5 milliseconds; continuously carrying out 200 times of detonation and detonation pressure release treatment on the material; obtaining a black product in the reaction bin;
(5) Separation and drying: and (4) separating and drying the material obtained in the step (4) to obtain the expanded graphite.
The expanded graphite prepared by the embodiment has a remarkable diffraction peak at 2 theta =26.50 degrees, the lattice spacing is expanded to D =0.336nm, and the average thickness D =53.12nm.
Example 4
(1) Mixing materials: adding 20g of graphite powder into 20ml of water solution, and uniformly stirring;
(2) And (3) granulation: adding 1.25g of carboxymethyl cellulose emulsion (with the mass concentration of 5%) into the material obtained in the step (1) as a bonding agent, uniformly stirring the mixture into slurry, and preparing spherical particles with the diameter of 1cm, namely the micro honeycomb coal-shaped graphite spheres;
(3) And (3) drying: putting the material obtained in the step (2) into an electrothermal constant-temperature drying oven at 60 ℃ for drying for 40min until the water content is 3.8%;
(4) Continuous detonation: putting the material obtained in the step (3) into a closed container for detonation pressure release treatment, namely introducing saturated steam into the container to increase the pressure to 2MP, keeping the pressure for 60s, and releasing the pressure to the atmospheric pressure within 87.5 milliseconds; continuously carrying out 350 times of detonation and detonation pressure release treatment on the material; obtaining a black product in the reaction bin;
(5) Separation and drying: and (5) separating and drying the material obtained in the step (4) to obtain the expanded graphite.
The expanded graphite prepared by the embodiment has a remarkable diffraction peak at 2 theta =26.03 degrees, the lattice spacing is expanded to D =0.342nm, and the average thickness D =50.72nm.
Example 5
(1) Mixing materials: adding 20g of graphite powder into 20ml of absolute ethyl alcohol solution (with the mass concentration of 99.7 percent), and uniformly stirring;
(2) And (3) granulation: adding 1.8g of silicon rubber emulsion (mass concentration is 2%) into the material obtained in the step (1) as an adhesive, uniformly stirring the mixture into slurry, and preparing spherical particles with the diameter of 1cm, namely the micro honeycomb coal-shaped graphite spheres;
(3) And (3) drying: putting the material obtained in the step (2) into a 50 ℃ electric heating constant-temperature drying oven to be dried for 40min until the water content is 4.7%;
(4) Continuous detonation: putting the material obtained in the step (3) into a closed container for detonation pressure release treatment, namely introducing saturated steam into the container to increase the pressure to 2MP, keeping the pressure for 60s, and releasing the pressure to the atmospheric pressure within 87.5 milliseconds; continuously carrying out detonation pressure release treatment on the material for 500 times; obtaining a black product in the reaction bin;
(5) Separation and drying: and (4) separating and drying the material obtained in the step (4) to obtain the expanded graphite.
The expanded graphite prepared by the embodiment has a remarkable diffraction peak at 2 theta =25.86 degrees, the lattice spacing is expanded to D =0.344nm, and the average thickness D =50.08nm.
TABLE 1X-ray diffraction data sheet for various embodiments of the present invention
| Sample numbering | 2Theta(degree) | d(nm) | D(nm) |
| Graphite | 26.55 | 0.335 | 53.12 |
| Example 1 | 26.18 | 0.340 | 51.38 |
| Example 2 | 26.11 | 0.341 | 52.41 |
| Example 3 | 26.50 | 0.336 | 53.12 |
| Example 4 | 26.03 | 0.342 | 50.72 |
| Example 5 | 25.86 | 0.344 | 50.08 |
It should be understood that the above embodiments are merely exemplary embodiments adopted to illustrate the principle of the present invention, however, the present invention is not limited thereto, and specific embodiments may be determined according to the technical solutions and practical situations of the present invention. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit and substance of the invention, and such modifications and improvements added thereto are considered to be within the scope of the invention.
Claims (5)
1. A method for preparing expanded graphite by adopting a continuous detonation pressure release technology is characterized by comprising the following steps:
(1) Mixing materials: adding graphite powder into a proper amount of polar solvent to form a solid-liquid mixture, and uniformly stirring;
(2) And (3) granulation: adding a proper amount of adhesive into the material obtained in the step (1), and uniformly stirring the mixture into slurry to prepare spherical particles with the diameter of 1 cm;
(3) And (3) drying: drying the material obtained in the step (2) until the moisture content is 1-5%;
(4) Continuous detonation: putting the material obtained in the step (3) into a closed container for detonation pressure release treatment, namely introducing saturated steam into the container to increase the pressure to 0.5-2.5MPa, keeping the pressure for 50-180s, and releasing the pressure to the atmospheric pressure within 87 milliseconds by a flash opening mode of an end cover of the closed container; continuously carrying out detonation and detonation pressure release treatment on the material for multiple times;
(5) Separation and drying: and (5) separating and drying the material obtained in the step (4) to obtain the expanded graphite.
2. The method for preparing expanded graphite by continuous detonation pressure release technology according to claim 1, wherein the polar solvent in step (1) comprises water, alcohol or their mixture.
3. The method for preparing expanded graphite according to claim 1, wherein the binder in step (2) comprises one of emulsifier OP-10, carboxymethyl cellulose, polyvinyl alcohol emulsion, polytetrafluoroethylene emulsion, and silicone rubber.
4. The method for preparing expanded graphite by continuous detonation pressure relief according to claim 1, wherein the material drying method in step (3) is to put the material into a drying oven, heat the material to 30-60 ℃, and dry the material for 30-60 min.
5. The method for preparing expanded graphite by continuous detonation pressure release technology according to claim 1, wherein the continuous detonation times in step (4) are 50-500.
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| CN101003369A (en) * | 2007-01-17 | 2007-07-25 | 大连理工大学 | Detonation method for preparing laminar Nano graphite powder |
| CN101456553A (en) * | 2007-12-11 | 2009-06-17 | 晟茂（青岛）先进材料有限公司 | Chemical processing method for preparing high quality inflatable graphite |
| CN106592308A (en) * | 2017-01-05 | 2017-04-26 | 新疆弘瑞达纤维有限公司 | Gas explosion processor |
| CN107200320A (en) * | 2017-07-21 | 2017-09-26 | 长沙紫宸科技开发有限公司 | A kind of method that expanded graphite or graphene are prepared with electrolytic aluminium waste cathode carbon |
| CN109704316A (en) * | 2019-02-27 | 2019-05-03 | 盐城师范学院 | A kind of water is that the Detonation Process of medium is protected to prepare graphene |
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| CN101003369A (en) * | 2007-01-17 | 2007-07-25 | 大连理工大学 | Detonation method for preparing laminar Nano graphite powder |
| CN101456553A (en) * | 2007-12-11 | 2009-06-17 | 晟茂（青岛）先进材料有限公司 | Chemical processing method for preparing high quality inflatable graphite |
| CN106592308A (en) * | 2017-01-05 | 2017-04-26 | 新疆弘瑞达纤维有限公司 | Gas explosion processor |
| CN107200320A (en) * | 2017-07-21 | 2017-09-26 | 长沙紫宸科技开发有限公司 | A kind of method that expanded graphite or graphene are prepared with electrolytic aluminium waste cathode carbon |
| CN109704316A (en) * | 2019-02-27 | 2019-05-03 | 盐城师范学院 | A kind of water is that the Detonation Process of medium is protected to prepare graphene |
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