CN111470508A - Carbon compounding method of biological silicon monoxide and product thereof - Google Patents

Carbon compounding method of biological silicon monoxide and product thereof Download PDF

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CN111470508A
CN111470508A CN202010116919.2A CN202010116919A CN111470508A CN 111470508 A CN111470508 A CN 111470508A CN 202010116919 A CN202010116919 A CN 202010116919A CN 111470508 A CN111470508 A CN 111470508A
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CN111470508B (en
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金之坚
张学臣
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Shanghai Henglun Silicon Material Co ltd
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Shanghai Henglun New Energy Technology Co ltd
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Abstract

The invention discloses a carbon compounding method of biological silicon monoxide, which comprises the following steps: the method comprises the following steps: wet grinding the biological silicon oxide material, washing the ground biological silicon oxide material for a plurality of times by using deionized water, and drying the washed biological silicon oxide material; step two: vacuum mixing the dried biological silicon oxide material with high-temperature asphalt particles with the particle size of 1-10 mu m for later use; step three: and (4) introducing mixed gas of acetylene and inert gas into the mixed particles obtained in the fifth step under the negative pressure condition, wherein the acetylene accounts for 1-5% of the mixed gas, heating at the rotating speed of 1-15 r/min until the temperature reaches 700 ℃, preserving the heat, and naturally cooling to obtain the coated carbon composite biological silicon protoxide material. The invention also discloses a product thereof. The invention can relieve the change of the silicon oxide material, is beneficial to forming a stable SEI film, improves the first charge-discharge efficiency (coulombic efficiency), and can be mixed with a graphite material in a large proportion for application.

Description

Carbon compounding method of biological silicon monoxide and product thereof
Technical Field
The invention relates to the field of preparation of silicon oxide, in particular to a carbon compounding method of biological silicon oxide and a product thereof.
Background
The development of new energy power becomes a common target of electric automobiles internationally, and as the most important part of the electric automobiles, the development of power lithium batteries is a hot spot which is hoped to be ascribed to, and is a key target for measuring market application of the electric automobiles.
The energy density of the lithium battery in the prior art can only reach 256Wh/kg, and the difference is still left from the starting target of the power lithium battery 300Wh/kg established by the state.
In the prior art, new development and application of the anode material are continuously provided, so that the anode has greater technical advantages.
The silicon-carbon composite negative electrode material can increase the energy storage space of the negative electrode material, but at the same time, because the mineral silicon material almost has 300% of expansion phenomenon during the charging and discharging of the lithium battery, the silicon material on the surface of a current collector is peeled off, the cycle number is reduced, and the energy of the lithium battery is reduced.
Therefore, the existing silicon-carbon composite anode material is difficult to be applied to the anode material in a large proportion.
Disclosure of Invention
In order to overcome the above-mentioned drawbacks of the prior art, it is an object of the present invention to provide a method for carbon recombination of bio-silica and a product thereof.
In order to realize the purpose of the invention, the adopted technical scheme is as follows:
a carbon compounding method of biological silicon monoxide comprises the following steps:
the method comprises the following steps: wet crushing the biological silicon oxide material to reach the grain size of 0.05-10 microns, washing the biological silicon oxide material with deionized water for several times, and drying the biological silicon oxide material;
step two: vacuum mixing the dried biological silicon oxide material with high-temperature asphalt particles with the particle size of 1-10 mu m for later use;
step three: and (4) introducing mixed gas of acetylene and inert gas into the mixed particles obtained in the fifth step under the negative pressure condition, wherein the acetylene accounts for 1-5% of the mixed gas, heating at the rotating speed of 1-15 r/min until the temperature reaches 700 ℃, preserving the heat, and naturally cooling to obtain the coated carbon composite biological silicon protoxide material.
In a preferred embodiment of the invention, the biological silica material is SiOx, (0< X < 2).
In a preferred embodiment of the invention, the biological silica material is prepared by the following method:
the preparation method of the biological silicon dioxide coarse material comprises the following steps: cleaning rice hulls to remove heavy metals, and performing carbonization treatment and decarburization treatment to obtain a biological silicon dioxide coarse material;
the preparation method of the biological silicon dioxide comprises the following steps: crushing the crude biological silicon dioxide, soaking in 30-40% hydrochloric acid, soaking in pure water for several times, and vacuum drying to obtain biological silicon dioxide;
the preparation method of the biological silicon monoxide comprises the following steps: adopting a mixed gas of methane and high-purity hydrogen as a reduction medium, and carrying out deoxidation treatment on the biological silicon dioxide to obtain biological silicon monoxide, wherein the temperature of the deoxidation treatment is 1200-1400 ℃, and the biological silicon monoxide is SiOx (0< X < 2);
in a preferred embodiment of the present invention, the carbonization treatment in the crude bio-silica material preparation step is performed at a temperature ranging from 250 ℃ to 400 ℃ using a muffle furnace, and the decarburization treatment is performed at a temperature ranging from 400 ℃ to 900 ℃ using a tube furnace.
In a preferred embodiment of the present invention, the pulverization treatment in the bio-silica production step is to pulverize the bio-silica coarse material to a particle size of 500 mesh to 2500 mesh; the concentration of hydrochloric acid is 36%; the hydrochloric acid soaking time is 2-6 hours; soaking in pure water for at least three times, each time for at least three hours; vacuum drying is carried out at 70 deg.C for 12 hr.
In a preferred embodiment of the invention, the ratio of methane in the mixed gas in the step of preparing the biological silicon oxide is 2-5%, in the deoxidation treatment, the air input is 0.21L-0.89L/min, the temperature is firstly increased to 1210-1400 ℃ at the heating rate of 10 ℃/min, the temperature is kept for 30-60 minutes, and then the biological silicon oxide is obtained by rapid temperature reduction.
In a preferred embodiment of the present invention, the amount of the high-temperature asphalt particles added in the second step is 2-5 t% of the dry biological silica material.
In a preferred embodiment of the present invention, the flow rate of the mixed gas in step three is 50sccm to 300 sccm.
In a preferred embodiment of the present invention, the temperature raising process in the third step is:
heating the tube furnace to 400 ℃ at the speed of 10 ℃/min, then heating to 600 ℃ at the speed of 4-5 ℃/min, and then heating to 700-800 ℃ at the speed of 1.5-2 ℃/min.
In a preferred embodiment of the invention, the heat preservation time in the third step is 2-8 hours, and the temperature is naturally reduced to below 100 ℃.
A carbon composite biological silicon oxide material is prepared by the method.
The invention has the beneficial effects that:
the carbon composite biological silicon oxide material prepared by the invention can relieve the change of the silicon oxide material, is beneficial to forming a stable SEI film, improves the first charge-discharge efficiency (coulombic efficiency), and can be mixed with a graphite material in a large proportion.
Drawings
FIG. 1 is an electron micrograph of a carbon-composite bio-silica according to example 1 of the present invention.
FIG. 2 is an electron microscope image 2 of the carbon composite biological silicon oxide of the present invention.
Detailed Description
The working principle of the invention is as follows:
the carbon composite biological silicon oxide is obtained by tightly coating a layer of carbon material on the surface of the biological silicon oxide, so that the conductive contact performance is improved, and the silicon oxide material can be isolated from the electrolyte in practical application.
Example 1
300g of biological silicon oxide material is put into a small-sized nano sand mill, and industrial ethanol is adopted as a lubricant to crush the material at the speed of 200 rpm-1000 rpm until the particle size reaches the standard of 0.05 mu m-10 mu m.
And repeatedly cleaning the mixture twice by using deionized water, and drying the mixture by using a small spray dryer.
Putting the dried biological silicon oxide material and high-temperature asphalt particles with the particle size of 1-10 mu m and the weight ratio of 2t percent of the silicon oxide material into a vacuum mixer, and mixing and processing for 0.5-4 hours.
And (2) putting the mixed material into a tubular furnace, pumping air in the tubular furnace to a negative pressure state by using a vacuum pump, and introducing mixed gas of acetylene and inert gas (nitrogen or argon) at a flow rate of 50-300 sccm, wherein the mixing ratio of the acetylene and the inert gas can be 1-5%, namely the acetylene accounts for 1-5% of the total air input.
Keeping the tube furnace at the rotating speed of 1 r-15 r/min, heating the tube furnace to 400 ℃ at the speed of 10 ℃/min, then heating to 600 ℃ at the speed of 4 ℃/min, finally heating to 700 ℃ at the speed of 2 ℃/min, then preserving heat for 4-8 hours, naturally cooling to the temperature below 100 ℃, opening the furnace door, taking out the processed material, finishing the coating process, and obtaining the product shown in figure 1.
Example 2
300g of biological silicon oxide material is put into a small-sized nano sand mill, and industrial ethanol is adopted as a lubricant to crush the material at the speed of 200 rpm-1000 rpm until the particle size reaches the standard of 0.05 mu m-10 mu m.
And repeatedly cleaning the mixture twice by using deionized water, and drying the mixture by using a small spray dryer.
And (2) putting the dried biological silicon oxide material and high-temperature asphalt particles with the particle size of 1-10 mu m and the weight ratio of 5t percent of the silicon oxide material into a vacuum mixer, mixing and processing for 1-5 hours, and putting the mixed material into a tubular furnace.
After the air in the tubular furnace is pumped to a negative pressure state by a vacuum pump, mixed gas of acetylene and inert gas (nitrogen or argon) is introduced at the flow rate of 50 sccm-300 sccm, the mixing ratio of the acetylene and the inert gas can be between 1% and 5%, namely the acetylene accounts for 1% to 5% of the total air input.
Keeping the tube furnace at the rotating speed of 1 r-15 r/min, heating the tube furnace to 400 ℃ at the speed of 10 ℃/min, then heating to 600 ℃ at the speed of 4 ℃/min, finally heating to 800 ℃ at the speed of 2 ℃/min, then preserving heat for 2-6 hours, naturally cooling to the temperature below 100 ℃, opening the furnace door, taking out the processed material, finishing the coating process, and obtaining the product shown in figure 2.
After the biological silicon monoxide is coated by carbon, the internal structure of the biological silicon monoxide is unchanged, and in practical application, the outer carbon shell improves the stability and the conductivity of the whole structure, relieves the change of a silicon monoxide material, is beneficial to forming a stable SEI film, improves the first charge-discharge efficiency (coulombic efficiency), can be mixed with a graphite material in a large proportion and is used in a negative electrode material of a lithium battery.
Table 1 shows a comparison of the carbon-composite bio-silica material of the present invention with a carbon-composite ordinary silica material.
Figure BDA0002391777060000051

Claims (10)

1. A carbon compounding method of biological silicon monoxide is characterized by comprising the following steps:
the method comprises the following steps: wet crushing the biological silicon oxide material to reach the grain size of 0.05-10 microns, washing the biological silicon oxide material with deionized water for several times, and drying the biological silicon oxide material;
step two: vacuum mixing the dried biological silicon oxide material with high-temperature asphalt particles with the particle size of 1-10 mu m for later use;
step three: and (4) introducing mixed gas of acetylene and inert gas into the mixed particles obtained in the fifth step under the negative pressure condition, wherein the acetylene accounts for 1-5% of the mixed gas, heating at the rotating speed of 1-15 r/min until the temperature reaches 700 ℃, preserving the heat, and naturally cooling to obtain the coated carbon composite biological silicon protoxide material.
2. The method of claim 1, wherein the bio-silicon oxide material is SiOx (0< X < 2).
3. The method for carbon recombination of bio-silica according to claim 1, wherein the bio-silica material is prepared by the following method:
the preparation method of the biological silicon dioxide coarse material comprises the following steps: cleaning rice hulls to remove heavy metals, and performing carbonization treatment and decarburization treatment to obtain a biological silicon dioxide coarse material;
the preparation method of the biological silicon dioxide comprises the following steps: crushing the crude biological silicon dioxide, soaking in 30-40% hydrochloric acid, soaking in pure water for several times, and vacuum drying to obtain biological silicon dioxide;
the preparation method of the biological silicon monoxide comprises the following steps: and (2) deoxidizing the biological silicon dioxide by using a mixed gas of methane and high-purity hydrogen as a reduction medium to obtain biological silicon monoxide, wherein the temperature of the deoxidation treatment is 1200-1400 ℃, and the biological silicon monoxide is SiOx (0< X < 2).
4. The method for carbon sequestration of bio-silica according to claim 1, wherein the carbonization treatment in the bio-silica raw material preparation step is performed at a temperature ranging from 250 ℃ to 400 ℃ using a muffle furnace, and the decarburization treatment is performed at a temperature ranging from 400 ℃ to 900 ℃ using a tube furnace.
5. The method for carbon sequestration of biogenic silica according to claim 1, wherein the pulverization in the biogenic silica production step is carried out by pulverizing the biogenic silica coarse material to a particle size of 500 mesh to 2500 mesh; the concentration of hydrochloric acid is 36%; the hydrochloric acid soaking time is 2-6 hours; soaking in pure water for at least three times, each time for at least three hours; vacuum drying is carried out at 70 deg.C for 12 hr.
6. The carbon recombination method of biological silicon oxide according to claim 1, wherein the ratio of methane in the mixed gas in the step of preparing biological silicon oxide is 2% -5%, the air input in the deoxidation treatment is 0.21L-0.89L/min, the temperature is first raised to 1210-1400 ℃ at a heating rate of 10 ℃/min and then is preserved for 30-60 minutes, and then the biological silicon oxide is obtained by rapid cooling.
7. The method for carbon recombination of bio-silica as claimed in claim 1, wherein the amount of the high temperature pitch particles added in the second step is 2 t% of the dry bio-silica material.
8. The method as claimed in claim 1, wherein the flow rate of the mixed gas in the third step is 50sccm to 300 sccm.
9. The method for carbon recombination of biological silicon monoxide according to claim 1, wherein the temperature raising treatment in the third step is:
heating the tubular furnace to 400 ℃ at the speed of 10 ℃/min, heating to 600 ℃ at the speed of 4-5 ℃/min, and heating to 700-800 ℃ at the speed of 1.5-2 ℃/min;
and in the third step, the heat preservation time is 2-8 hours, and the temperature is naturally reduced to be below 100 ℃.
10. A carbon composite biosilica material according to any one of claims 1 to 9, wherein the carbon composite biosilica material is prepared by the above method.
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Cited By (2)

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CN113178564A (en) * 2021-04-25 2021-07-27 陈庆 Silicon dioxide-carbon composite material and preparation method and application thereof
CN113437272A (en) * 2021-06-24 2021-09-24 湖南中科星城石墨有限公司 Silica material, treatment method thereof and secondary battery cathode

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