CN113528171A - Needle coke calcination process - Google Patents
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Abstract
The invention discloses a needle coke calcining process, which belongs to the technical field of needle coke production and is characterized in that a box-type furnace is used for calcining raw coke, and the process comprises a pretreatment process, a preheating and heating process, a buffer heating process, a high-temperature calcining process and a post-treatment heating process; the invention has the beneficial effects that: superior true density and particle strength are obtained.
Description
The technical field is as follows:
the invention belongs to the technical field of needle coke production, and particularly relates to a needle coke calcination process.
Background art:
the carbon product made from needle coke has high crystallinity, high purity, low ablation, and low CTE, and is therefore the main quality raw material for manufacturing high power electrodes and ultra-high power electrodes, and the quality of the needle coke determines the material properties of the electrodes.
The main performance indexes of the needle coke comprise true density, strength, resistivity, thermal expansion coefficient and the like, and indexes such as sulfur content, nitrogen content, ash content and the like have great influence on the performance of the electrode.
True density indicates the degree of densification and the crystal lattice of the needle cokeThe arrangement regularity is simultaneously represented and the calcination degree is simultaneously characterized, and the true density of the needle coke cooked coke is usually more than or equal to 2.13g/cm3. The S, N content of needle coke is the main cause of electrode gas expansion and crack generation, and the S content is less than or equal to 0.5 percent and the N content is less than or equal to 0.5 percent.
The prior needle coke calcining process is a rotary kiln and rotary bed process, and has the following defects: the yield of the needle coke is low, generally 70-75%; the calcined coke has poor granularity, the granularity index is more than 3.5mm and accounts for more than 30 percent, the granularity index is less than 1mm and is not more than 10 percent, and the tap density is 0.8g/cm3。
The national invention patent with the patent number of 201810989595.6 discloses a novel process for calcining needle coke by a pot furnace, which comprises the steps of calcining green coke by the pot furnace, loading the green coke into the pot furnace, using fuel gas to support combustion by the pot furnace, slowly heating and calcining the needle coke from top to bottom, staying in the furnace for 40-60 hours, and simultaneously increasing the particle strength and tap density without damaging the particle size in the process of calcining and rearranging the needle coke due to the action of self gravity.
Although the method has a certain improvement on the true density and the tap density, the phenomenon of insufficient particle strength of calcined coke still exists, and the particle strength and the true density of the calcined coke still need to be further improved.
The invention content is as follows:
in order to solve the problems and overcome the defects of the prior art, the invention provides a needle coke calcination process which can effectively solve the problems of insufficient particle strength and true density.
The specific technical scheme for solving the technical problems comprises the following steps: the needle coke calcining process is characterized in that a box furnace is utilized to calcine raw coke, and comprises a preheating temperature-rising process, a buffering temperature-rising process and a high-temperature calcining process;
the preheating and temperature rising process comprises the steps of rising the temperature of the pretreated raw coke from 450 ℃ at a temperature rising speed of 2 ℃/min to 1000 ℃ and keeping the temperature for 1 h;
the buffer heating procedure comprises heating at a speed of 5 ℃/min from 1000 ℃ to 1350 ℃ and keeping the temperature for 1 h;
the high-temperature calcination procedure comprises the steps of heating up from 1350 ℃ at the heating-up speed of 2 ℃/min, and keeping the temperature for 1h after the temperature reaches 1400 ℃.
Further, the preheating and temperature raising process also comprises a pretreatment process, wherein the pretreatment process comprises the step of raising the temperature of the green coke from room temperature to 450 ℃ at a temperature raising speed of 10 ℃/min.
Furthermore, the box-type furnace is heated by adopting a silicon-molybdenum rod, the temperature measuring thermocouple is wrapped and protected by adopting corundum, and the box-type furnace is operated by adopting an intermittent production mode.
Furthermore, the box furnace is operated in a positive pressure heating mode of intermittent production, and the pressure is 20-500 pa.
Further, the positive pressure heating mode of the batch production is as follows: injecting argon from 4 gas injection points of the box furnace before the pretreatment process, replacing air in a hearth with argon, wherein the air inflow of the argon is 2-10m3/h。
Further, the high-temperature calcination process also comprises a post-treatment temperature rise process, wherein the post-treatment temperature rise process rises from 1400 ℃ of the high-temperature calcination process at a temperature rise speed of 2 ℃/min, and the temperature is kept for 1h after the temperature reaches 1450 ℃.
Further, the high-temperature calcination process also comprises a post-treatment temperature rise process, wherein the post-treatment temperature rise process rises from 1400 ℃ of the high-temperature calcination process at a temperature rise speed of 2 ℃/min, and after reaching 1450 ℃, the temperature is reduced by 10 ℃/min to 1350 ℃, and then the temperature is raised to 1450 ℃ according to 2 ℃/min, and the temperature is kept constant for 1 h.
The invention has the beneficial effects that:
(1) the temperature is increased from room temperature to 450 ℃ in a gradient manner, so that the fiber structure of the needle coke can be protected, the large-diameter pores on the surface of the needle coke are reduced, the true density of the needle coke is improved, the crystal surface structure of the needle coke is improved, the needle coke has excellent true density, the microcosmic carbon layer surface area is parallelized, the surface spacing is reduced, and the needle coke is easier to graphitize;
(2) the invention adopts the buffer heating process, avoids the problems that the box-type furnace adopts a silicon-molybdenum rod for intermittent heating, the heating element and the temperature measuring thermocouple have expansion and contraction phenomena in a specific temperature region, the heating element and the temperature measuring thermocouple are deformed, bent and broken, the service life is shortened, and the load of other heating regions is suddenly increased after the heating element or the temperature measuring thermocouple is broken, so that the product quality is finally influenced;
(3) the invention keeps the temperature at the node of 1400 ℃ for 1h, and unexpectedly finds that the nitrogen content of calcined coke can be effectively reduced, the true density of the calcined coke is further improved, the rupture strength and the electric conductivity of the ultrahigh-power electrode are favorably improved, and the thermal expansion coefficient of the ultrahigh-power electrode is reduced;
(4) the post-treatment heating procedure adopts a cooling means, improves the particle strength of calcined coke, further improves the true density of the calcined coke, solves the problem of insufficient particle strength of the calcined coke in the traditional calcining process, and particularly ensures the realization of the effects by combining the pretreatment procedure with the post-treatment heating procedure.
Description of the drawings:
FIG. 1 is a photograph of a burnt polarization photograph of comparative example 1 of the present invention after calcination;
FIG. 2 is a photograph of a burnt polarization photograph of example 1 of the present invention;
FIG. 3 is a structural view of a box-type furnace of comparative example 3 of the present invention;
FIG. 4 is a structural view of a box-type furnace according to example 1 of the present invention.
The specific implementation mode is as follows:
in the description of the invention, specific details are given only to enable a full understanding of the embodiments of the invention, but it should be understood by those skilled in the art that the invention is not limited to these details for the implementation. In other instances, well-known structures and functions have not been described or shown in detail to avoid obscuring the points of the embodiments of the invention. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
The specific implementation mode of the invention is as follows:
example 1:
the needle coke calcining process includes calcining green coke in a box furnace, injecting argon from 4 gas injecting points in the box furnace to replace air inside the hearth with argon in the amount of 2-10m3H, heating by adopting a silicon-molybdenum rod in a box furnace, and performing thermocouple temperature measurementWrapping and protecting with corundum, operating in a positive pressure heating mode of intermittent production at a pressure of 20-500pa, and including a pretreatment process, a preheating and heating process, a buffer heating process, a high-temperature calcination process and a post-treatment heating process;
the pretreatment procedure comprises the step of heating the green coke from room temperature to 450 ℃ at a heating rate of 10 ℃/min;
the preheating and temperature rising process comprises the steps of rising the temperature of the pretreated raw coke from 450 ℃ at a temperature rising speed of 2 ℃/min to 1000 ℃ and keeping the temperature for 1 h;
the buffer heating procedure comprises heating at a speed of 5 ℃/min from 1000 ℃ to 1350 ℃ and keeping the temperature for 1 h;
the high-temperature calcination procedure comprises the steps of heating up from 1350 ℃ at the heating-up speed of 2 ℃/min, and keeping the temperature for 1h after the temperature reaches 1400 ℃.
The post-treatment temperature rise procedure raises the temperature from 1400 ℃ of the high-temperature calcination procedure at the temperature rise speed of 2 ℃/min, and keeps the temperature for 1h after the temperature reaches 1450 ℃.
And after the needle coke is calcined, cooling, increasing the air input, naturally cooling to below 100 ℃, closing the air source, and discharging.
Example 2 as another example:
the needle coke calcining process includes calcining green coke in a box furnace, injecting argon from 4 gas injecting points in the box furnace to replace air inside the hearth with argon in the amount of 2-10m3Heating by adopting a silicon-molybdenum rod in a box-type furnace, wrapping and protecting a temperature measuring thermocouple by adopting corundum, operating by adopting a positive pressure heating mode of intermittent production, wherein the pressure is 20-500pa, and operating comprises a pretreatment process, a preheating and heating process, a buffering and heating process, a high-temperature calcination process and a post-treatment and heating process;
the pretreatment procedure comprises the step of heating the green coke from room temperature to 450 ℃ at a heating rate of 10 ℃/min;
the preheating and temperature rising process comprises the steps of rising the temperature of the pretreated raw coke from 450 ℃ at a temperature rising speed of 2 ℃/min to 1000 ℃ and keeping the temperature for 1 h;
the buffer heating procedure comprises heating at a speed of 5 ℃/min from 1000 ℃ to 1350 ℃ and keeping the temperature for 1 h;
the high-temperature calcination procedure comprises the steps of heating up from 1350 ℃ at the heating-up speed of 2 ℃/min, and keeping the temperature for 1h after the temperature reaches 1400 ℃.
The post-treatment temperature rise procedure is to raise the temperature from 1400 ℃ of the high-temperature calcination procedure at a temperature rise speed of 2 ℃/min to 1450 ℃, then to lower the temperature to 1350 ℃ at a speed of 10 ℃/min, and then to raise the temperature to 1450 ℃ at a speed of 2 ℃/min, and to keep the temperature constant for 1 h.
And after the needle coke is calcined, cooling, increasing the air input, naturally cooling to below 100 ℃, closing the air source, and discharging.
In order to more intuitively show the advantages of the pretreatment process, the pretreatment process method adopted by the invention is compared with the equivalent replacement method adopted by the same process,
comparative example 1:
the procedure is as in example 1, except that: in the preparation process of the comparative example, the pretreatment process is adopted, the moisture content of the green coke is less than or equal to 3 percent after the green coke is dried by high-temperature flue gas at 800 ℃,
comparative example 2:
the procedure is as in example 1, except that: in the preparation process of the comparative example, the pretreatment process is adopted, the moisture content of the green coke is less than or equal to 3 percent after the green coke is dried by high-temperature flue gas at 450 ℃,
the test results are as follows:
table 1: effect of different pretreatment processes on calcined coke product quality
| Process of treatment | Sample name | Sulfur content% | Nitrogen content% | Volatile content% | Water content% | Ash content% | True density g/cm3 | |
| Example 1 | Gradient heating from room temperature to 450 DEG C | Calcined coke | 0.2 | 0.37 | 0.35 | 0.1 | 0.1 | 2.16 |
| Comparative example 1 | Directly heating to 800 DEG C | Calcined coke | 0.21 | 0.37 | 0.5 | 0.1 | 0.12 | 2.14 |
| Comparative example 2 | Directly heating to 450 DEG C | Calcined coke | 0.2 | 0.36 | 0.47 | 0.1 | 0.12 | 2.141 |
From the data analysis in table 1, it can be seen that:
the temperature is increased from room temperature to 450 ℃ in a gradient manner, so that the fiber structure of the needle coke can be protected, the large-diameter pores on the surface of the needle coke are reduced, the true density of the needle coke is improved, the crystal surface structure of the needle coke is improved, the needle coke has excellent true density, the microcosmic carbon layer surface area is parallelized, the surface spacing is reduced, and the needle coke is easier to graphitize. From the two groups of polarization micrographs, the fiber structure is well preserved by the treatment of gradient temperature rise between room temperature and 450 ℃, the true density of calcined coke is improved to 2.16, and the volatile content is reduced to 0.35 percent.
The reason for this is that the temperature is directly raised to 450 or 800 ℃, moisture and volatile components are largely released, the fiber structure of the needle coke is damaged, the large-diameter pores on the surface of the coke are reduced, and the crystal face structure of the needle coke is improved. As can be seen from the polarized photographs, the calcined coke pores directly heated to 800 ℃ are more, the fiber structure is greatly damaged, and the fiber structure has low true density and high volatile component.
In order to more intuitively show the process advantages of the buffer heating procedure of the invention, the buffer heating procedure method is compared with the equivalent replacement method adopted by the same process,
comparative example 3:
the procedure is as in example 1, except that: in the preparation process of the comparative example, the buffer heating procedure is modified to directly heat to 1400 ℃;
comparative example 4:
the procedure is as in example 1, except that: in the preparation process of the comparative example, the buffer heating procedure is cancelled; and the box furnace is replaced by a rotary kiln or a rotary bed;
comparative example 5:
the procedure is as in example 1, except that: in the preparation process of the comparative example, the buffer heating procedure is cancelled; and the box-type furnace is replaced by a tank-type furnace with negative pressure;
specifically, the green coke is heated to 450 ℃ from room temperature at a heating rate of 10 ℃/min; the water content is less than or equal to 3 percent, the raw coke enters a pre-calcining bin through bucket lifting, the material is cooled to be below 100 ℃, the raw coke is lifted to a tank furnace top distributing machine through a pre-calcining feeding bucket and then is automatically fed to each tank furnace, the temperature of the pretreated raw coke is increased from 450 ℃ at the temperature increasing speed of 2 ℃/min through adjusting the negative pressure of each flame path, and the temperature is kept for 1 hour after the temperature reaches 1000 ℃; heating up from 1000 ℃ at a heating rate of 2 ℃/min, and keeping the temperature for 1h after the temperature reaches 1400 ℃; heating up to 1400 ℃ at the heating rate of 2 ℃/min, and keeping the temperature for 1h after reaching 1450 ℃.
The present invention and comparative examples 3-5 show that:
the box-type furnace adopts a silicon-molybdenum rod for heating, the temperature measuring thermocouple adopts corundum for wrapping protection, belongs to intermittent production and needs frequent temperature rise and fall, and the heating element and the temperature measuring thermocouple have expansion and contraction phenomena in a specific temperature area, which is shown in the attached drawing 3 in detail; in the similar calcining equipment, a rotary furnace and a pot furnace do not have the phenomenon.
As comparative examples 4 and 5 for comparison, the rotary kiln, the rotary bed or the pot furnace does not have frequent temperature rise and fall, and the heating element and the temperature measuring thermocouple do not have expansion and contraction phenomena in a specific temperature region, so that the equipment is not greatly influenced by the elimination of the buffer temperature rise process.
In comparison example 3, the box-type furnace is heated by a silicon-molybdenum rod, and is operated in a positive pressure heating mode of intermittent production, the heating element and the temperature measuring thermocouple are greatly damaged by directly heating to 1400 ℃, so that the heating element and the temperature measuring thermocouple are deformed, bent and broken, the service life is shortened, and after the heating element or the temperature measuring thermocouple is broken, the load of other heating areas is suddenly increased, and the product quality is finally influenced, which is shown in an attached figure 4.
In order to more intuitively show the technological advantages of the high-temperature calcination procedure, the invention is characterized in that a buffer heating procedure method is compared with an equivalent replacement method adopted by the same technology,
comparative example 6:
the procedure is as in example 1, except that: in the preparation process of the comparative example, the high-temperature calcination procedure is replaced by heating from 1350 ℃ at a heating rate of 2 ℃/min, and the temperature is kept for 1h after reaching 1450 ℃.
Table 2: influence of different high-temperature calcination procedures on the quality of calcined coke products
| Sample name | Sulfur content% | Nitrogen content% | Volatile content% | Water content% | Ash content% | True density g/cm3 | |
| Example 1 | Calcined coke | 0.2 | 0.37 | 0.35 | 0.1 | 0.1 | 2.16 |
| Comparative example 6 | Calcined coke | 0.2 | 0.51 | 0.32 | 0.06 | 0.15 | 2.145 |
According to the data analysis, the following results are obtained: as can be seen from the table, after 1350-,
in contrast, in comparative example 6, the temperature is directly raised to 1450 ℃, and the content of nitrogen in calcined coke exceeds the standard, so that the phenomenon of crystal expansion occurs in the manufacturing process of the ultrahigh-power graphite electrode, the electrode cracks, and the product is unqualified;
the temperature is kept for 1h at a node of 1400 ℃, and the method is unexpectedly found to effectively reduce the nitrogen content of calcined coke, further improve the true density of the calcined coke, be beneficial to improving the breaking strength and the electrical conductivity of the ultrahigh-power electrode and reduce the thermal expansion coefficient of the ultrahigh-power electrode.
In order to more intuitively show the process advantages of the post-treatment temperature-rising procedure of the invention, the invention is compared with the embodiment 1 and the embodiment 2,
table 3: influence of different post-treatment heating procedures on the quality of calcined coke products
| Sample name | Sulfur content% | Nitrogen content% | Volatile content% | Water content% | Ash content% | True density g/cm3 | Strength of the granules% | |
| Example 2 | Calcined coke | 0.14 | 0.35 | 0.32 | 0.08 | 0.09 | 2.175 | 33.6 |
| Example 1 | Calcined coke | 0.2 | 0.37 | 0.35 | 0.1 | 0.1 | 2.16 | 29.6 |
According to the data analysis, the following results are obtained: as can be seen from the table, in example 2, the post-treatment temperature-raising step employs a temperature-lowering means, and the true density is increased from 2.16g/cm3 to 2.175g/cm3, and particularly the particle strength is increased from 29.6% to 33.6%.
Thus, the problem that the strength of calcined coke particles in the traditional calcining process is insufficient is solved, the particle strength of calcined coke is improved, and the true density of calcined coke is further improved.
In order to more intuitively show the process advantages of the influence of the pretreatment process on the post-treatment temperature-rising process, the following steps are compared with example 1 and example 2,
comparative example 7:
the preparation method is the same as example 2, except that: the pretreatment process is adopted, the raw coke is directly heated to 450 ℃, after the high-temperature flue gas is dried, the water content is less than or equal to 3 percent,
table 4: influence of pretreatment process on post-treatment heating process
| Sample name | Sulfur content% | Nitrogen content% | Volatile content% | Water content% | Ash content% | True density g/cm3 | Strength of the granules% | |
| Example 1 | Calcined coke | 0.2 | 0.37 | 0.35 | 0.1 | 0.1 | 2.16 | 29.6 |
| Example 2 | Calcined coke | 0.14 | 0.35 | 0.32 | 0.08 | 0.09 | 2.175 | 33.6 |
| Comparative example 7 | Calcined coke | 0.21 | 0.37 | 0.4 | 0.2 | 0.12 | 2.159 | 27.1 |
According to the data analysis, the following results are obtained:
in comparative example 7, the temperature was lowered in the post-treatment temperature-raising step, but the grain strength was only 27.1%, which was lower than 29.6% in example 1 without the post-treatment temperature-raising step,
this is probably because the green coke is directly heated to 450 ℃, moisture and volatile components are greatly escaped, the fiber structure of the needle coke is damaged, the large-diameter pores on the coke surface are reduced, the fiber structure of the needle coke cannot resist the strength of the cooling means, but the fiber structure of the needle coke is further damaged, and the final particle strength is only 27.1%.
In summary, the following steps:
(1) the temperature is increased from room temperature to 450 ℃ in a gradient manner, so that the fiber structure of the needle coke can be protected, the large-diameter pores on the surface of the needle coke are reduced, the true density of the needle coke is improved, the crystal surface structure of the needle coke is improved, the needle coke has excellent true density, the microcosmic carbon layer surface area is parallelized, the surface spacing is reduced, and the needle coke is easier to graphitize;
(2) the invention adopts the buffer heating process, avoids the problems that the box-type furnace adopts a silicon-molybdenum rod for intermittent heating, the heating element and the temperature measuring thermocouple have expansion and contraction phenomena in a specific temperature region, the heating element and the temperature measuring thermocouple are deformed, bent and broken, the service life is shortened, and the load of other heating regions is suddenly increased after the heating element or the temperature measuring thermocouple is broken, so that the product quality is finally influenced;
(3) the invention keeps the temperature at the node of 1400 ℃ for 1h, and unexpectedly finds that the nitrogen content of calcined coke can be effectively reduced, the true density of the calcined coke is further improved, the rupture strength and the electric conductivity of the ultrahigh-power electrode are favorably improved, and the thermal expansion coefficient of the ultrahigh-power electrode is reduced;
(4) the post-treatment heating procedure adopts a cooling means, improves the particle strength of calcined coke, further improves the true density of the calcined coke, solves the problem of insufficient particle strength of the calcined coke in the traditional calcining process, and particularly ensures the realization of the effects by combining the pretreatment procedure with the post-treatment heating procedure.
Claims (7)
1. A needle coke calcining process is characterized in that a box furnace is used for calcining green coke, and comprises a preheating temperature-rising process, a buffering temperature-rising process and a high-temperature calcining process;
the preheating and temperature rising process comprises the steps of rising the temperature of the pretreated raw coke from 450 ℃ at a temperature rising speed of 2 ℃/min to 1000 ℃ and keeping the temperature for 1 h;
the buffer heating procedure comprises heating at a speed of 5 ℃/min from 1000 ℃ to 1350 ℃ and keeping the temperature for 1 h;
the high-temperature calcination procedure comprises the steps of heating up from 1350 ℃ at the heating-up speed of 2 ℃/min, and keeping the temperature for 1h after the temperature reaches 1400 ℃.
2. The needle coke calcination process of claim 1, wherein the preheating step further comprises a pretreatment step comprising heating the green coke from room temperature to 450 ℃ at a heating rate of 10 ℃/min.
3. The needle coke calcination process according to claim 2, wherein the box furnace is heated by a silicon-molybdenum rod, the temperature thermocouple is coated and protected by corundum, and the process is operated in an intermittent production mode.
4. The needle coke calcination process of claim 3, wherein the box furnace is operated with a batch production positive pressure heating mode, the pressure being 20-500 pa.
5. The needle coke calcination process of claim 4, wherein the batch production positive pressure heating mode is: injecting argon from 4 gas injection points of the box furnace before the pretreatment process, replacing air in a hearth with argon, wherein the air inflow of the argon is 2-10m3/h。
6. The needle coke calcination process according to claim 4, wherein the high-temperature calcination process further comprises a post-treatment temperature-raising process, wherein the post-treatment temperature-raising process raises the temperature from 1400 ℃ of the high-temperature calcination process at a temperature-raising rate of 2 ℃/min, and maintains the temperature for 1h after reaching 1450 ℃.
7. The needle coke calcination process according to claim 4, wherein the high-temperature calcination process further comprises a post-treatment temperature-raising process, wherein the post-treatment temperature-raising process raises the temperature from 1400 ℃ of the high-temperature calcination process at a temperature-raising speed of 2 ℃/min, lowers the temperature to 1350 ℃ at a speed of 10 ℃/min after reaching 1450 ℃, then raises the temperature to 1450 ℃ at a speed of 2 ℃/min, and keeps the temperature for 1 hour.
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|---|
| 李和言等: "《装甲车辆制造工艺学》", 30 June 2019, 北京理工大学出版社 * |
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