CN113999010B - Preparation method of high-performance special graphite - Google Patents
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- CN113999010B CN113999010B CN202111525799.2A CN202111525799A CN113999010B CN 113999010 B CN113999010 B CN 113999010B CN 202111525799 A CN202111525799 A CN 202111525799A CN 113999010 B CN113999010 B CN 113999010B
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Abstract
The invention discloses a preparation method of high-performance special graphite, relates to the technical field of graphite preparation, and aims to solve the problems that raw material powder and asphalt are not uniformly kneaded and coated enough and the asphalt is excessive; the method comprises grinding calcined petroleum coke, sieving into different size fractions, weighing appropriate amount of raw material powder of each size fraction, and mixing; selecting medium-temperature coal pitch as a binder; preheating raw material powder, melting medium-temperature coal pitch, respectively spraying the raw material powder and pitch through two nozzles, enabling the raw material powder to pass through a pitch spraying path and fall outside the pitch spraying path end point, coating the pitch on the surface of the raw material powder, respectively collecting redundant pitch and the raw material powder coated with the pitch, and cooling to obtain paste; grinding the paste, winnowing and profiling, and then sequentially carrying out primary roasting, dipping, secondary roasting and graphitization to obtain a graphite product; the raw material powder and the asphalt have good coating effect, the product performance is excellent, and the consumption of the asphalt is saved.
Description
Technical Field
The invention relates to the technical field of graphite preparation, in particular to a preparation method of high-performance special graphite.
Background
The special graphite is a high-strength, high-density and high-purity graphite product, is widely applied to the industrial fields of metallurgy, chemical industry, aerospace, electronics, machinery, nuclear energy and the like, and particularly has high requirements on the special graphite in some special fields, and the traditional graphite production method is difficult to meet the requirements and needs to be improved in some aspects.
The production process of graphite mainly comprises raw material grinding, kneading, sheet rolling, paste grinding, multiple roasting, dipping, graphitization and the like, and for example, the method is disclosed in an invention patent with the publication number of CN101823707A and the name of 'a process method for producing isostatic pressing graphite'; however, the quality of the graphite product is directly determined by the quality of the kneading process, the traditional kneading process is to mix the raw material powder and the asphalt at high temperature, so that the raw material powder is coated by the asphalt as much as possible, the raw material powder particles are fine and are easy to gather together among the particles, the surfaces of some particles are difficult to coat the asphalt in the kneading process, and even if the surfaces of the material particles are coated by the asphalt, the coating amount is also extremely uneven, so that the particles cannot be effectively bonded, and the performance of the graphite product is reduced. Secondly, because the coating amount cannot be controlled, asphalt is almost used excessively in the traditional kneading process, the performance of graphite products is reduced due to excessive asphalt, and asphalt is wasted. Therefore, a method for preparing high-performance special graphite is needed to solve the problem.
Disclosure of Invention
The invention aims to provide a preparation method of high-performance special graphite, which aims to solve the problems that the raw material powder and asphalt are not uniformly kneaded and coated enough and the asphalt is excessive.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of high-performance special graphite comprises the following specific steps:
s1, grinding calcined petroleum coke, screening into different size fractions, weighing a proper amount of raw material powder of each size fraction, and uniformly mixing; selecting medium-temperature coal pitch as a binder;
s2, preheating raw material powder, melting medium-temperature coal pitch, respectively spraying the raw material powder and pitch through two nozzles, enabling the raw material powder to pass through a pitch spraying path and fall outside the end point of the pitch spraying path, coating the pitch on the surface of the raw material powder, respectively collecting redundant pitch and the raw material powder coated with the pitch, and cooling to obtain a paste;
s3, placing the paste into a ball milling tank, grinding, taking out, and winnowing to obtain paste powder with a large specific gravity;
s4, uniformly mixing the paste powder, filling the mixture into a mold, and profiling to obtain a green body;
and S5, sequentially carrying out primary roasting, dipping, secondary roasting and graphitization on the green body to obtain a graphite product.
In an optimal scheme in the step S2, the two nozzles respectively form a certain included angle with the horizontal plane, a paste material collecting table is arranged below an intersection point of the two spraying paths and used for collecting raw material powder wrapped with asphalt, and a vertical distance from the intersection point to the paste material collecting table is not less than two meters.
In the scheme, the nozzle and the ground form an angle of 30-60 degrees, and the spraying direction is inclined downwards.
In the scheme, the nozzles for spraying the asphalt are flat, the sprayed asphalt is in a liquid level shape, and the liquid level is perpendicular to the vertical plane where the central points of the two nozzles are located.
In a preferred embodiment of step S1, the raw material powder includes, by weight, 50 to 70 parts of 0.074mm grade, 10 to 30 parts of 0.074 to 0.15mm grade, 10 to 20 parts of 0.15 to 0.5mm grade, and 5 to 10 parts of 0.5 to 1.0mm grade.
In an advantageous embodiment of step S1, the medium temperature coal tar pitch has a softening point of 100 to 200 ℃.
In an advantageous embodiment of step S2, the raw material powder is preheated to 100-200 ℃ and the temperature of the molten asphalt is 150-280 ℃.
In a preferred scheme in the step S3, the ball milling medium is stainless steel balls with the diameter of 2.0mm, and the grinding time is 2-10 min; the wind speed of the air separation is 5-20 m/s.
In an advantageous embodiment of step S4, the pressing is extrusion, molding or isostatic pressing, the pressure is 180-280 MPa, and the pressing time is 5-30 min.
In an optimal scheme in the step S5, the roasting maximum temperature is 800-1000 ℃, and the heating rate is 2-10 ℃/h; the impregnant is low-temperature coal pitch, the softening point of the impregnant is 80-160 ℃, the impregnation temperature is 200-280 ℃, the impregnation time is 2-10 h, the impregnation pressure is 2-5 Mpa, the graphitization highest temperature is 2600-3000 ℃, and the heating rate is 10-60 ℃/h.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the preparation method of the high-performance special graphite, the raw material powder and the asphalt liquid are intersected and sprayed at a certain angle, so that the raw material powder passes through a spraying path of the asphalt liquid, asphalt is uniformly coated on the surface of the raw material powder in the process, a good coating effect is achieved, excessive asphalt in raw materials and products is avoided, the using amount of the asphalt is reduced, the cost is saved, and meanwhile, the performance improvement of graphite products is greatly promoted.
2. According to the preparation method of the high-performance special graphite, the raw material powder is preheated before spray coating is carried out, so that the interparticle polymerization effect is reduced, asphalt is coated on the surfaces of particle materials as much as possible, and a better coating effect is achieved.
3. According to the preparation method of the high-performance special graphite, the paste collecting table is arranged at a certain fall below the intersection point of the raw material powder and the asphalt spraying, so that the raw material powder coated with asphalt liquid can be naturally cooled, and the preparation flow is further shortened.
4. The preparation method of the high-performance special graphite is characterized in that materials wrapping the asphalt are ground properly, and part of the adhered asphalt can be stripped off, so that the amount of the asphalt in a product is further reduced, the particle sphericity is facilitated, and the performance of the graphite product is facilitated.
5. According to the preparation method of the high-performance special graphite, the asphalt and the light materials with lighter specific gravity are removed by adopting an air separation sieve, so that the density and the uniformity of the raw materials are ensured, and the performance of the graphite product is effectively improved.
6. The preparation method of the high-performance special graphite optimizes the process parameters of the procedures of material preparation, compression, roasting, impregnation, graphitization and the like to adapt to the novel process without kneading, flaking and secondary grinding, and provides guarantee for the stability of product performance.
Detailed Description
The preparation method of the high-performance special graphite comprises the following steps:
firstly grinding calcined petroleum coke, sieving the ground petroleum coke into different size fractions, preferably sieving four material with the size fractions of less than 0.074mm, 0.074-0.15 mm, 0.15-0.5 mm and 0.5-1.0 mm, weighing a proper amount of raw material powder of each size fraction, and uniformly mixing, wherein the weighed raw material powder is preferably 50-70 parts of 0.074mm fraction, 10-30 parts of 0.074-0.15 mm fraction, 10-20 parts of 0.15-0.5 mm fraction and 5-10 parts of 0.5-1.0 mm fraction in parts by weight under the preferable sieving scheme;
selecting medium-temperature coal pitch as a binder, heating to melt the binder, wherein the softening point of the medium-temperature coal pitch is preferably 100-200 ℃, the melting temperature of the medium-temperature coal pitch is preferably 150-280 ℃, preheating raw material powder to reduce the interparticle polymerization effect, so that the asphalt is coated on the surface of as many granular materials as possible, the preheating temperature is preferably 100-200 ℃, respectively spraying the raw material powder and the asphalt through two nozzles, enabling the raw material powder to pass through an asphalt spraying path and fall outside the end point of the asphalt spraying path, coating the asphalt on the surface of the raw material powder, respectively collecting redundant asphalt and the raw material powder coated with the asphalt, cooling to obtain paste, and heating to melt the asphalt collected at the end point of the asphalt spraying path for continuous use;
in a preferred embodiment, the two nozzles respectively form a certain included angle with the horizontal plane, preferably 30-60 degrees, the spraying direction is inclined downwards, a paste collecting table is arranged below the intersection point of the two spraying paths and used for collecting the raw material powder coated with the asphalt, the vertical distance from the intersection point to the paste collecting table is not less than two meters, and the height difference is set so as to enable the raw material powder coated with the asphalt to be naturally cooled in the falling process; furthermore, the nozzles for spraying the asphalt can be flat, so that the sprayed asphalt is in a liquid surface shape, and the liquid surface is perpendicular to a vertical plane where the central points of the two nozzles are located, so that the raw material powder can be sprayed to the flowing liquid surface and passes through the liquid surface after being coated with the asphalt, and the complicated operation that the linear spraying needs an accurate path is reduced;
in addition, the two nozzles are respectively connected with a feeding machine, and the feeding speed is controlled to adjust the spraying speed;
then the paste is put into a ball milling tank for grinding, part of the asphalt which is not firmly bonded is peeled off, meanwhile, the paste is shaped to have better sphericity, preferably, the ball milling medium is stainless steel balls with the diameter of 2.0mm, the grinding time is 2-10 min, the paste is taken out for air separation after grinding, redundant asphalt and particles with smaller volume or lower density are screened out by controlling the air speed, and paste powder with larger specific gravity is obtained, wherein the air speed is preferably 5-20 m/s in the preferred embodiment;
uniformly mixing the paste powder, putting the mixture into a mold, and pressing to obtain a green body, wherein the pressing can be extrusion, mold pressing or isostatic pressing, the pressure is preferably 180-280 Mpa, and the pressing time is preferably 5-30 min;
finally, sequentially carrying out primary roasting, dipping, secondary roasting and graphitization on the green body to obtain a graphite product, wherein in a preferred embodiment, the roasting maximum temperature is 800-1000 ℃, and the heating rate is 2-10 ℃/h; the impregnant is low-temperature coal pitch, the softening point of the impregnant is 80-160 ℃, the impregnation temperature is 200-280 ℃, the impregnation time is 2-10 h, the impregnation pressure is 2-5 Mpa, the graphitization highest temperature is 2600-3000 ℃, and the heating rate is 10-60 ℃/h.
Example 1
(1) Preparing raw materials: grinding the calcined petroleum coke, sieving into four grades of materials with the grain sizes of less than 0.074mm, 0.074-0.15 mm, 0.15-0.5 mm and 0.5-1.0 mm, and respectively taking 50 parts, 30 parts, 20 parts and 10 parts of the four grades of materials.
(2) And (3) asphalt coating: the petroleum coke powder is mixed evenly and preheated to 150 ℃, and simultaneously the asphalt is melted at 200 ℃. Respectively spraying the raw material powder and the asphalt liquid through a nozzle, keeping the two spraying directions to form 50-degree angles with the ground, and collecting the coated raw material powder as a paste for later use;
(3) Paste processing: and (3) placing the paste into a ball milling tank for grinding for 5min, taking out the material, and then winnowing in a winnowing machine with the wind speed of 10m/s to obtain paste powder with a large specific gravity.
(4) Profiling: mixing the paste powder obtained by air separation, placing in a rubber sleeve, and isostatic pressing for 6min at 180 MPa.
(5) Roasting, dipping and graphitizing: sequentially roasting the formed green body at the highest temperature of 900 ℃, the heating rate of 6 ℃/h, keeping the temperature at the highest temperature for 5h, then impregnating, wherein the impregnant is low-temperature coal pitch, the softening point of the impregnant is 80-160 ℃, the impregnation temperature is 250 ℃, the impregnation time is 2h, the impregnation pressure is 2Mpa, then carrying out secondary roasting, the roasting at the highest temperature of 850 ℃, the heating rate of 10 ℃/h, keeping the temperature at the highest temperature for 5h, finally graphitizing, wherein the graphitizing at the highest temperature of 2900 ℃, the heating rate of 20 ℃/h, and keeping the temperature at the highest temperature for 5h.
The graphite prepared by the method has high performance and the bulk density is 1.88g/cm 3 Compressive strength of 67.4MPa, fracture resistanceStrength 31.5MPa, resistivity 7.8 mu omega m, thermal expansion coefficient 2.72 x 10 at 500 DEG C -6 /° c, and each has a good isotropy.
Example 2
(1) Preparing raw materials: grinding the calcined petroleum coke, sieving into four grades of materials with the grain sizes of less than 0.074mm, 0.074-0.15 mm, 0.15-0.5 mm and 0.5-1.0 mm, and respectively taking 70 parts, 15 parts, 10 parts and 5 parts of the four grades of materials.
(2) And (3) asphalt coating: the petroleum coke powder is mixed evenly and preheated to 200 ℃, and meanwhile, the asphalt is melted at 250 ℃. Respectively spraying the raw material powder and the asphalt liquid through a nozzle, keeping the two spraying directions to form an angle of 60 degrees with the ground, and collecting the coated raw material powder as a paste for later use;
(3) Paste processing: and (3) placing the paste into a ball milling tank for grinding for 8min, taking out the material, and then winnowing in a winnowing machine with the air speed of 20m/s to obtain paste powder with a large specific gravity.
(4) Profiling: and (3) uniformly mixing the paste powder obtained by air separation, placing the mixture into a rubber sleeve, and carrying out isostatic pressing, wherein the forming pressure is 220MPa, and the forming time is 30min.
(5) Roasting, dipping and graphitizing: sequentially roasting the molded green body for one time, wherein the roasting maximum temperature is 1000 ℃, the heating rate is 8 ℃/h, keeping the temperature at the maximum temperature for 5h, then impregnating, the impregnant adopts low-temperature coal pitch, the softening point is 80-160 ℃, the impregnating temperature is 280 ℃, the impregnating time is 5h, the impregnating pressure is 3Mpa, then carrying out secondary roasting, the roasting maximum temperature is 900 ℃, the heating rate is 10 ℃/h, keeping the temperature at the maximum temperature for 5h, finally graphitizing, the graphitizing maximum temperature is 3000 ℃, the heating rate is 60 ℃/h, and keeping the temperature at the maximum temperature for 5h.
The graphite prepared by the method has high performance and the bulk density is 1.90g/cm 3 Compressive strength of 73.7MPa, flexural strength of 34.2MPa, resistivity of 8.91 mu omega m, and thermal expansion coefficient of 2.94 x 10 at 500 DEG C -6 /° c, and each has a good isotropy.
Example 3
(1) Preparing raw materials: grinding the calcined petroleum coke, sieving into four grades of materials with the grain sizes of less than 0.074mm, 0.074-0.15 mm, 0.15-0.5 mm and 0.5-1.0 mm, and respectively taking 60 parts, 25 parts, 10 parts and 5 parts of the four grades of materials.
(2) And (3) asphalt coating: mixing petroleum coke powder uniformly and preheating to 200 ℃, and melting asphalt at 280 ℃. Respectively spraying the raw material powder and the asphalt liquid through a nozzle, keeping the two spraying directions to form an angle of 40 degrees with the ground, and collecting the coated raw material powder as a paste for later use;
(3) Processing of paste: and (3) placing the paste into a ball milling tank for grinding for 10min, taking out the material, and then winnowing in a winnowing machine with the wind speed of 15m/s to obtain paste powder with a large specific gravity.
(4) Profiling: and (3) uniformly mixing the paste powder obtained by air separation, placing the mixture into a rubber sleeve, and performing isostatic pressing, wherein the molding pressure is 280MPa, and the molding time is 15min.
(5) Roasting, dipping and graphitizing: sequentially roasting the molded green body for one time, wherein the roasting maximum temperature is 950 ℃, the heating rate is 4 ℃/h, keeping the temperature at the maximum temperature for 5h, then impregnating, the impregnant adopts low-temperature coal pitch, the softening point is 80-160 ℃, the impregnating temperature is 280 ℃, the impregnating time is 8h, the impregnating pressure is 5Mpa, then carrying out secondary roasting, the roasting maximum temperature is 950 ℃, the heating rate is 6 ℃/h, keeping the temperature at the maximum temperature for 5h, finally graphitizing, the graphitizing maximum temperature is 2700 ℃, the heating rate is 30 ℃/h, and keeping the temperature at the maximum temperature for 5h.
The graphite prepared by the method has high performance and the bulk density is 1.92g/cm 3 Compressive strength of 85.8MPa, flexural strength of 40.0MPa, resistivity of 9.33 mu omega m, and thermal expansion coefficient of 3.16 x 10 at 500 DEG C -6 /° c, and each has a good isotropy.
From the three embodiments, the graphite prepared by the preparation method of the high-performance special graphite has excellent performances in all aspects, particularly has outstanding bulk density performance, and can be applied to various special fields.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are also included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope defined by the claims.
The present invention is not described in detail, but is known to those skilled in the art.
Claims (10)
1. The preparation method of the high-performance special graphite is characterized by comprising the following specific steps of:
s1, grinding calcined petroleum coke, screening into different size fractions, weighing a proper amount of raw material powder of each size fraction, and uniformly mixing; selecting medium-temperature coal pitch as a binder;
s2, preheating raw material powder, melting medium-temperature coal pitch, respectively spraying the raw material powder and pitch through two nozzles, enabling the sprayed pitch to be liquid-surface-shaped, enabling the liquid surface to be perpendicular to a vertical plane where the central points of the two nozzles are located, enabling the raw material powder to penetrate through a pitch spraying path and fall outside the end point of the pitch spraying path, enabling the surface of the raw material powder to be coated with the pitch, respectively collecting redundant pitch and the raw material powder coated with the pitch, and cooling to obtain a paste;
s3, placing the paste into a ball milling tank, grinding, taking out, and winnowing to obtain paste powder with a large specific gravity;
s4, uniformly mixing the paste powder, filling the mixture into a mold, and profiling to obtain a green body;
and S5, sequentially carrying out primary roasting, dipping, secondary roasting and graphitization on the green body to obtain a graphite product.
2. A preparation method of high-performance special graphite according to claim 1, characterized by comprising the following steps: in the step S2, the two nozzles respectively form a certain included angle with the horizontal plane, a paste collecting table is arranged below the intersection point of the two spraying paths and used for collecting raw material powder wrapped with asphalt, and the vertical distance from the intersection point to the paste collecting table is not less than two meters.
3. The preparation method of the special high-performance graphite as claimed in claim 2, wherein the preparation method comprises the following steps: the angle between the nozzle and the ground is 30-60 degrees, and the spraying direction is inclined downwards.
4. The preparation method of the special high-performance graphite as claimed in claim 3, wherein the preparation method comprises the following steps: the nozzle for spraying the asphalt is flat.
5. The preparation method of the special high-performance graphite as claimed in claim 1, wherein the preparation method comprises the following steps: in the step S1, the raw material powder weighed comprises, by weight, 50-70 parts of 0.074mm grade, 10-30 parts of 0.074-0.15 mm grade, 10-20 parts of 0.15-0.5 mm grade and 5-10 parts of 0.5-1.0 mm grade.
6. The preparation method of the special high-performance graphite as claimed in claim 1, wherein the preparation method comprises the following steps: in the step S1, the softening point of the medium-temperature coal pitch is 100-200 ℃.
7. A preparation method of high-performance special graphite according to claim 1, characterized by comprising the following steps: in the step S2, the raw material powder is preheated to 100-200 ℃, and the temperature of the molten asphalt is 150-280 ℃.
8. The preparation method of the special high-performance graphite as claimed in claim 1, wherein the preparation method comprises the following steps: in the step S3, the ball milling medium is a stainless steel ball with the diameter of 2.0mm, and the grinding time is 2-10 min; the wind speed of the air separation is 5-20 m/s.
9. A preparation method of high-performance special graphite according to claim 1, characterized by comprising the following steps: in the step S4, the compression molding is extrusion, die pressing or isostatic pressing, the pressure is 180-280 Mpa, and the compression molding time is 5-30 min.
10. The preparation method of the special high-performance graphite as claimed in claim 1, wherein the preparation method comprises the following steps: in the step S5, the roasting highest temperature is 800-1000 ℃, and the heating rate is 2-10 ℃/h; the impregnant is low-temperature coal pitch, the softening point of the impregnant is 80-160 ℃, the impregnation temperature is 200-280 ℃, the impregnation time is 2-10 h, the impregnation pressure is 2-5 Mpa, the graphitization highest temperature is 2600-3000 ℃, and the heating rate is 10-60 ℃/h.
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CN115215655A (en) * | 2022-08-09 | 2022-10-21 | 中钢集团南京新材料研究院有限公司 | Kneading method of isostatic pressing graphite product and product thereof |
CN116200046A (en) * | 2023-02-21 | 2023-06-02 | 滑县鑫进碳素销售有限公司 | High-temperature coal tar pitch |
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