Carbonaceous material, method for producing the same, and use thereof

By optimizing the raw material composition and preparation process of carbonaceous materials, a simplified preparation of high-performance sealing materials has been achieved, solving the problems of complex processes and high energy consumption in existing technologies, improving material performance and reducing costs.

CN119591404BActive Publication Date: 2026-01-06ZIGONG DONGXIN CARBON CO LTD
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Patent Information

Application Number
CN202411759760.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-12-03
Publication Date
2026-01-06
Estimated Expiration
2044-12-03

AI Technical Summary

Technical Problem

The existing carbonaceous sealing materials have complex and energy-intensive manufacturing processes, which cannot meet the high performance and reliability requirements of modern industry for sealing materials.

Method used

Carbonaceous materials are prepared by using a specific ratio of coke powder, graphite, carbon black and modified pitch as raw materials through a single calcination process. By controlling the content of coke powder with different volatiles and adjusting the type of graphite, the parameters in the preparation process, such as dry mixing, closed mixing, rolling and calcination temperature, are optimized, and the preparation process is simplified.

Benefits of technology

It improves the open porosity, flexural strength, compressive strength and Shore hardness of carbonaceous materials, reduces preparation costs and simplifies the process.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application provides a carbonaceous material and a preparation method and application thereof, and relates to the technical field of carbon material processing.The carbonaceous material comprises, in percentage by mass, 30-45% of coke powder, 25-30% of graphite, 3.5-8% of carbon black and 26.5-33% of pitch; the coke powder is composed of coke powder containing 1-2% of volatile matter and coke powder containing 8-14% of volatile matter; the graphite is microcrystalline graphite and T395 graphite powder; and the pitch is modified pitch containing 45-60% of volatile matter.The carbonaceous material has the characteristics of low porosity, high bending strength and compressive strength and moderate Shore hardness after one-time baking, the preparation method is simple, efficient and low in cost, and the carbonaceous material has a wide application prospect.
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Description

Technical Field

[0001] This invention provides a carbonaceous material, its preparation method, and its application, relating to the field of carbon material processing technology. Background Technology

[0002] Sealing materials are essential for preventing oil, gas, and water leaks, as well as preventing the intrusion of external environmental media and dust, in industries such as electromechanical products, petroleum, and chemicals. Modern industry places increasingly higher demands on the reliability of seals, but traditional sealing materials each have a series of problems and cannot meet the requirements of modern industry.

[0003] Chinese patent CN106672959A discloses a high-performance sealing material and its production process. The raw materials are modified coke powder, graphite powder, and asphalt in a weight ratio of 36-50:12.5-36:28-37.5. The modified coke powder is obtained after special pretreatment. The carbon-graphite sealing material has a bulk density reaching [missing information].

[0004] Its strength is 1.68-1.78 g / cm3, its flexural strength is 65-85 MPa, and its compressive strength is 180-250 MPa. However, its preparation process requires calcining the coke powder once, and then adding other raw materials for calcination once more, making the preparation process complex and energy-intensive.

[0005] Chinese patent CN108821770A discloses a method for preparing a high-performance graphite sealing material. This method involves mixing ultrafine coke powder with a particle size below 10 μm, graphite powder with a particle size below 50 μm, and pitch coke powder with a particle size below 50 μm. Then, medium-temperature pitch with a softening point of 70℃-100℃ and a residual carbon content of 30wt%-50wt% is added. After mixing and kneading, the mixture is rolled into sheets, cooled, crushed, and ground to form pressed powder. This powder is then pressed into shape using a ring-shaped molding die, and the ring-shaped preform is placed in a sealed crucible and fired 2-3 times. This method involves numerous firing cycles, high energy consumption, and a complex process. Summary of the Invention

[0006] This invention addresses the problems existing in the prior art by providing a carbonaceous material, its preparation method, and its application. This carbonaceous material has high open porosity, flexural strength, compressive strength, and Shore hardness, and requires only one calcination. The preparation method is simple and efficient.

[0007] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0008] On one hand, the present invention provides a carbonaceous material comprising, by mass percentage: 30-45% coke powder, 25-30% graphite, 3.5-8% carbon black and 26.5-33% pitch; wherein the coke powder is composed of coke powder containing 1-2% volatile matter and coke powder containing 8-14% volatile matter; wherein the graphite is microcrystalline graphite and T395 graphite powder; and wherein the pitch is modified pitch with 45-60% volatile matter.

[0009] Furthermore, the carbon black is N330 carbon black.

[0010] Furthermore, the mass ratio of the coke powder containing 1-2% volatile matter to the coke powder containing 8-14% volatile matter is 1.5-2.5:0.8-1.

[0011] Furthermore, the coke powder containing 1-2% volatile matter has a passing rate of 80-90% on a 320-mesh sieve.

[0012] Furthermore, the coke powder containing 8-14% volatile matter has a particle size of D50: 5-10 μm.

[0013] Preferably, the carbonaceous material comprises, by mass percentage: 37-40% coke powder, 25-28.5% graphite, 4-6% carbon black and 28-30% pitch.

[0014] Preferably, the carbonaceous material comprises, by mass percentage: 38.6% coke powder, 28.5% graphite, 4.2% carbon black and 28.7% pitch.

[0015] Preferably, the mass ratio of coke powder containing 0.26%-0.55% volatile matter to coke powder containing 10-14% volatile matter is 1.5-2.5:1.

[0016] Preferably, the mass ratio of the coke powder containing 1-2% volatile matter to the coke powder containing 8-14% volatile matter is 2:1.

[0017] Furthermore, the mass ratio of the microcrystalline graphite to T395 graphite powder is 4-5:0.5-1.

[0018] Preferably, the mass ratio of the microcrystalline graphite to T395 graphite powder is 5:0.5-1.

[0019] Preferably, the mass ratio of the microcrystalline graphite to T395 graphite powder is 5:0.7.

[0020] Furthermore, the microcrystalline graphite has a 320-mesh sieve pass rate of 80-85%.

[0021] Furthermore, the T395 graphite powder has a 320-mesh sieve passing rate of 75-85%.

[0022] Furthermore, the pH of the T395 graphite powder is 7.

[0023] Secondly, the present invention provides a method for preparing carbonaceous materials, the specific steps of which include:

[0024] S1. Dry mix coke powder, graphite and carbon black, add modified asphalt, and mix in a closed manner to obtain a paste. Roll the paste into a roll to obtain a sheet.

[0025] S2. Grind the rolled sheet obtained in step S1 into powder, stir and mix evenly to obtain fine powder;

[0026] S3. Pour the fine powder obtained in step S2 into a mold and press it to obtain the coarse product;

[0027] S4. Roast the crude product obtained in step S3.

[0028] S5. Remove from the oven after cooling.

[0029] Further, the fine powder in step S2 has a moisture content of 0-1 wt%, a volatile content of 12-18 wt%, and a sieve particle size of 1-5 wt% above a 160-mesh sieve and 55-60 wt% below a 320-mesh sieve.

[0030] Furthermore, the dry mixing conditions described in step S1 are: dry mixing at 110-130℃ for 60-90 minutes.

[0031] Furthermore, the closed-mixing conditions described in step S1 are: closed mixing at 170-180℃ for 90 minutes.

[0032] Furthermore, the temperature of the rolls in step S1 is 170-200℃.

[0033] Furthermore, the thickness of the rolled sheet in step S1 is 2-4 mm.

[0034] Furthermore, the pressing conditions described in step S3 are: a single pressure of 200-220 MPa and a holding time of 2-5 seconds.

[0035] Further, the density of the crude product in step S3 is 1.5 ± 0.03 g / cm³. 3 .

[0036] Further, the roasting conditions described in step S4 are as follows: the temperature is increased from room temperature to 250-280℃ at a rate of 45-50℃ / h, then increased to 450-500℃ at a rate of 1-2℃ / h, then increased to 700-750℃ at a rate of 2-3℃ / h, then increased to 850-900℃ at a rate of 4-5℃ / h, then increased to 1100-1200℃ at a rate of 5-10℃ / h, and then held at 1100-1200℃ for 60-70 hours before the furnace is shut down.

[0037] Thirdly, the present invention provides a carbonaceous sealing material, comprising the above-mentioned carbonaceous material or the carbonaceous material prepared by the above-mentioned preparation method.

[0038] Fourthly, the present invention provides a bearing comprising the above-described carbonaceous material or the carbonaceous material prepared by the above-described preparation method.

[0039] Fifthly, the present invention provides an apparatus comprising the aforementioned carbonaceous sealing material or the aforementioned bearing.

[0040] Sixthly, the present invention provides an application of carbonaceous materials and their preparation methods in reducing product costs.

[0041] The technical effects achieved by this invention are:

[0042] (1) This invention improves various properties of carbonaceous materials, including open porosity, flexural strength, compressive strength and Shore hardness, by controlling the content of different volatile coke powders in the raw materials, adjusting the content of different types of graphite and adjusting the type of carbon black.

[0043] (2) By controlling the amount of different raw materials and various parameters of fine powder during the preparation process, including moisture, volatile matter and particle size, the present invention enables carbonaceous materials to achieve high performance level with only one calcination, which simplifies the preparation method and saves costs. Detailed Implementation

[0044] To make the technical means, creative features, achieved objectives, and effects of this invention readily understandable, the invention is further illustrated below with reference to specific embodiments. However, the following embodiments are merely preferred embodiments of this invention and not all embodiments. Other embodiments obtained by those skilled in the art based on the embodiments described herein without creative effort are all within the protection scope of this invention. The technical and scientific terms used in the embodiments have meanings commonly understood by those skilled in the art to which this invention pertains.

[0045] The present invention does not limit the source of the raw materials used. Unless otherwise specified, the raw materials used in the present invention are all commercially available products in this technical field. The following is an exemplary description.

[0046]

[0047]

[0048] I. Examples and Comparative Examples

[0049] Coke powder with 1-2% volatile matter is called coke powder A, and coke powder with 8-14% volatile matter is called coke powder B.

[0050] Example 1

[0051] The bill of materials for Example 1 is shown in Table 1.

[0052] Table 1

[0053]

[0054] Preparation method:

[0055] S1. Dry mix coke powder, graphite and carbon black at 110℃ for 60 minutes, add modified asphalt, and close mix at 170℃ for 90 minutes to obtain a paste. Roll the paste at 170℃ to obtain a 2mm thick sheet.

[0056] S2. Grind the rolled sheet obtained in step S1 into powder, stir and mix evenly to obtain fine powder;

[0057] S3. Pour the fine powder obtained in step S2 into a mold and press it to obtain the coarse product;

[0058] S4. Roast the crude product obtained in step S3.

[0059] S5. Remove from the oven after cooling.

[0060] The roasting curve is as follows: the temperature is increased from room temperature to 280℃ at 50℃ / h, then increased to 500℃ at 1℃ / h, then increased to 750℃ at 2.5℃ / h, then increased to 900℃ at 5℃ / h, then increased to 1200℃ at 10℃ / h, and then held at 1200℃ for 68 hours before the furnace is shut down.

[0061] The fine powder obtained in step S2 has the following characteristics: moisture content of 0.2 wt%, volatile matter of 12 wt%, and particle size distribution: 1 wt% fine powder above a 160-mesh sieve and 55 wt% fine powder below a 320-mesh sieve.

[0062] Example 2

[0063] The bill of materials for Example 2 is shown in Table 2.

[0064] Table 2

[0065]

[0066] Preparation method:

[0067] S1. Dry mix coke powder, graphite and carbon black at 130℃ for 90 minutes, add modified asphalt, and close mix at 180℃ for 90 minutes to obtain a paste. Roll the paste at 200℃ to obtain a 4mm thick sheet.

[0068] S2. Grind the rolled sheet obtained in step S1 into powder, stir and mix evenly to obtain fine powder;

[0069] S3. Pour the fine powder obtained in step S2 into a mold and press it to obtain the coarse product;

[0070] S4. Roast the crude product obtained in step S3.

[0071] S5. Remove from the oven after cooling.

[0072] The roasting curve is as follows: the temperature is increased from room temperature to 280℃ at 50℃ / h, then increased to 500℃ at 1℃ / h, then increased to 750℃ at 2.5℃ / h, then increased to 900℃ at 5℃ / h, then increased to 1200℃ at 10℃ / h, and then held at 1200℃ for 68 hours before the furnace is shut down.

[0073] The fine powder obtained in step S2 has the following characteristics: moisture content of 1 wt%, volatile matter of 18 wt%, and particle size distribution: 5 wt% fine powder above 160 mesh and 60 wt% fine powder below 320 mesh.

[0074] Example 3

[0075] The bill of materials for Example 3 is shown in Table 3.

[0076] Table 3

[0077]

[0078]

[0079] Preparation method:

[0080] S1. Dry mix coke powder, graphite and carbon black at 110℃ for 60 minutes, add modified asphalt, and close mix at 170℃ for 90 minutes to obtain a paste. Roll the paste at 170℃ to obtain a 3mm thick sheet.

[0081] S2. Grind the rolled sheet obtained in step S1 into powder, stir and mix evenly to obtain fine powder;

[0082] S3. Pour the fine powder obtained in step S2 into a mold and press it to obtain the coarse product;

[0083] S4. Roast the crude product obtained in step S3.

[0084] S5. Remove from the oven after cooling.

[0085] The roasting curve is as follows: the temperature is increased from room temperature to 280℃ at 50℃ / h, then increased to 500℃ at 1℃ / h, then increased to 750℃ at 2.5℃ / h, then increased to 900℃ at 5℃ / h, then increased to 1200℃ at 10℃ / h, and then held at 1200℃ for 68 hours before the furnace is shut down.

[0086] The fine powder obtained in step S2 has the following characteristics: moisture content of 0.2 wt%, volatile matter of 12 wt%, and particle size distribution: 1 wt% fine powder above a 160-mesh sieve and 55 wt% fine powder below a 320-mesh sieve.

[0087] Comparative Example 1

[0088] The difference from Example 3 is that Comparative Example 1, by mass percentage, includes: 29% coke powder, 23% graphite, 12% carbon black and 36% pitch, as shown in Table 4.

[0089] Table 4

[0090]

[0091] Preparation method:

[0092] S1. Dry mix coke powder, graphite and carbon black at 110℃ for 60 minutes, add modified asphalt, and close mix at 170℃ for 90 minutes to obtain a paste. Roll the paste at 170℃ to obtain a 3mm thick sheet.

[0093] S2. Grind the rolled sheet obtained in step S1 into powder, stir and mix evenly to obtain fine powder;

[0094] S3. Pour the fine powder obtained in step S2 into a mold and press it to obtain the coarse product;

[0095] S4. Roast the crude product obtained in step S3.

[0096] S5. Remove from the oven after cooling.

[0097] The roasting curve is as follows: the temperature is increased from room temperature to 280℃ at 50℃ / h, then increased to 500℃ at 1℃ / h, then increased to 750℃ at 2.5℃ / h, then increased to 900℃ at 5℃ / h, then increased to 1200℃ at 10℃ / h, and then held at 1200℃ for 68 hours before the furnace is shut down.

[0098] The fine powder obtained in step S2 has the following characteristics: moisture content of 0.2 wt%, volatile matter of 12 wt%, and particle size distribution: 1 wt% fine powder above a 160-mesh sieve and 55 wt% fine powder below a 320-mesh sieve.

[0099] Comparative Example 2

[0100] The difference from Example 3 is that coke powder A is replaced by coke powder A' with 1% volatile matter, and coke powder B is replaced by coke powder B' with 7% volatile matter. The material list of Comparative Example 2 is shown in Table 5.

[0101] Table 5

[0102]

[0103] Preparation method:

[0104] S1. Dry mix coke powder, graphite and carbon black at 110℃ for 60 minutes, add modified asphalt, and close mix at 170℃ for 90 minutes to obtain a paste. Roll the paste at 170℃ to obtain a 3mm thick sheet.

[0105] S2. Grind the rolled sheet obtained in step S1 into powder, stir and mix evenly to obtain fine powder;

[0106] S3. Pour the fine powder obtained in step S2 into a mold and press it to obtain the coarse product;

[0107] S4. Roast the crude product obtained in step S3.

[0108] S5. Remove from the oven after cooling.

[0109] The roasting curve is as follows: the temperature is increased from room temperature to 280℃ at 50℃ / h, then increased to 500℃ at 1℃ / h, then increased to 750℃ at 2.5℃ / h, then increased to 900℃ at 5℃ / h, then increased to 1200℃ at 10℃ / h, and then held at 1200℃ for 68 hours before the furnace is shut down.

[0110] The fine powder obtained in step S2 has the following characteristics: moisture content of 0.2 wt%, volatile matter of 12 wt%, and particle size distribution: 1 wt% fine powder above a 160-mesh sieve and 55 wt% fine powder below a 320-mesh sieve.

[0111] Comparative Example 3

[0112] Compared with Example 3, Comparative Example 3 only used microcrystalline graphite. The bill of materials for Comparative Example 3 is shown in Table 6.

[0113] Table 6

[0114]

[0115] Preparation method:

[0116] S1. Dry mix coke powder, graphite and carbon black at 110℃ for 60 minutes, add modified asphalt, and close mix at 170℃ for 90 minutes to obtain a paste. Roll the paste at 170℃ to obtain a 3mm thick sheet.

[0117] S2. Grind the rolled sheet obtained in step S1 into powder, stir and mix evenly to obtain fine powder;

[0118] S3. Pour the fine powder obtained in step S2 into a mold and press it to obtain the coarse product;

[0119] S4. Roast the crude product obtained in step S3.

[0120] S5. Remove from the oven after cooling.

[0121] The roasting curve is as follows: the temperature is increased from room temperature to 280℃ at 50℃ / h, then increased to 500℃ at 1℃ / h, then increased to 750℃ at 2.5℃ / h, then increased to 900℃ at 5℃ / h, then increased to 1200℃ at 10℃ / h, and then held at 1200℃ for 68 hours before the furnace is shut down.

[0122] The fine powder obtained in step S2 has the following characteristics: moisture content of 0.2 wt%, volatile matter of 12 wt%, and particle size distribution: 1 wt% fine powder above a 160-mesh sieve and 55 wt% fine powder below a 320-mesh sieve.

[0123] Comparative Example 4

[0124] Compared with Example 3, Comparative Example 4 only used T395 graphite powder. The material list of Comparative Example 4 is shown in Table 7.

[0125] Table 7

[0126]

[0127] Preparation method:

[0128] S1. Dry mix coke powder, graphite and carbon black at 110℃ for 60 minutes, add modified asphalt, and close mix at 170℃ for 90 minutes to obtain a paste. Roll the paste at 170℃ to obtain a 3mm thick sheet.

[0129] S2. Grind the rolled sheet obtained in step S1 into powder, stir and mix evenly to obtain fine powder;

[0130] S3. Pour the fine powder obtained in step S2 into a mold and press it to obtain the coarse product;

[0131] S4. Roast the crude product obtained in step S3.

[0132] S5. Remove from the oven after cooling.

[0133] The roasting curve is as follows: the temperature is increased from room temperature to 280℃ at 50℃ / h, then increased to 500℃ at 1℃ / h, then increased to 750℃ at 2.5℃ / h, then increased to 900℃ at 5℃ / h, then increased to 1200℃ at 10℃ / h, and then held at 1200℃ for 68 hours before the furnace is shut down.

[0134] The fine powder obtained in step S2 has the following characteristics: moisture content of 0.2 wt%, volatile matter of 12 wt%, and particle size distribution: 1 wt% fine powder above a 160-mesh sieve and 55 wt% fine powder below a 320-mesh sieve.

[0135] Comparative Example 5

[0136] The difference from Example 3 is that T395 graphite powder was replaced with T295 graphite powder in Comparative Example 5. The material list of Comparative Example 5 is shown in Table 8.

[0137] Table 8

[0138]

[0139] Preparation method:

[0140] S1. Dry mix coke powder, graphite and carbon black at 110℃ for 60 minutes, add modified asphalt, and close mix at 170℃ for 90 minutes to obtain a paste. Roll the paste at 170℃ to obtain a 3mm thick sheet.

[0141] S2. Grind the rolled sheet obtained in step S1 into powder, stir and mix evenly to obtain fine powder;

[0142] S3. Pour the fine powder obtained in step S2 into a mold and press it to obtain the coarse product;

[0143] S4. Roast the crude product obtained in step S3.

[0144] S5. Remove from the oven after cooling.

[0145] The roasting curve is as follows: the temperature is increased from room temperature to 280℃ at 50℃ / h, then increased to 500℃ at 1℃ / h, then increased to 750℃ at 2.5℃ / h, then increased to 900℃ at 5℃ / h, then increased to 1200℃ at 10℃ / h, and then held at 1200℃ for 68 hours before the furnace is shut down.

[0146] The fine powder obtained in step S2 has the following characteristics: moisture content of 0.2 wt%, volatile matter of 12 wt%, and particle size distribution: 1 wt% fine powder above a 160-mesh sieve and 55 wt% fine powder below a 320-mesh sieve.

[0147] Comparative Example 6

[0148] Compared with Example 3, Comparative Example 6 replaced N330 carbon black with N220 carbon black. The material list of Comparative Example 6 is shown in Table 9.

[0149] Table 9

[0150]

[0151] Preparation method:

[0152] S1. Dry mix coke powder, graphite and carbon black at 110℃ for 60 minutes, add modified asphalt, and close mix at 170℃ for 90 minutes to obtain a paste. Roll the paste at 170℃ to obtain a 3mm thick sheet.

[0153] S2. Grind the rolled sheet obtained in step S1 into powder, stir and mix evenly to obtain fine powder;

[0154] S3. Pour the fine powder obtained in step S2 into a mold and press it to obtain the coarse product;

[0155] S4. Roast the crude product obtained in step S3.

[0156] S5. Remove from the oven after cooling.

[0157] The roasting curve is as follows: the temperature is increased from room temperature to 280℃ at 50℃ / h, then increased to 500℃ at 1℃ / h, then increased to 750℃ at 2.5℃ / h, then increased to 900℃ at 5℃ / h, then increased to 1200℃ at 10℃ / h, and then held at 1200℃ for 68 hours before the furnace is shut down.

[0158] The fine powder obtained in step S2 has the following characteristics: moisture content of 0.2 wt%, volatile matter of 12 wt%, and particle size distribution: 1 wt% fine powder above a 160-mesh sieve and 55 wt% fine powder below a 320-mesh sieve.

[0159] Comparative Example 7

[0160] The difference from Example 3 is that the mass ratio of coke powder A to coke powder B is 2.5:0.5. The material list for Comparative Example 7 is shown in Table 10.

[0161] Table 10

[0162]

[0163] Preparation method:

[0164] S1. Dry mix coke powder, graphite and carbon black at 110℃ for 60 minutes, add modified asphalt, and close mix at 170℃ for 90 minutes to obtain a paste. Roll the paste at 170℃ to obtain a 3mm thick sheet.

[0165] S2. Grind the rolled sheet obtained in step S1 into powder, stir and mix evenly to obtain fine powder;

[0166] S3. Pour the fine powder obtained in step S2 into a mold and press it to obtain the coarse product;

[0167] S4. Roast the crude product obtained in step S3.

[0168] S5. Remove from the oven after cooling.

[0169] The roasting curve is as follows: the temperature is increased from room temperature to 280℃ at 50℃ / h, then increased to 500℃ at 1℃ / h, then increased to 750℃ at 2.5℃ / h, then increased to 900℃ at 5℃ / h, then increased to 1200℃ at 10℃ / h, and then held at 1200℃ for 68 hours before the furnace is shut down.

[0170] The fine powder obtained in step S2 has the following characteristics: moisture content of 0.2 wt%, volatile matter of 12 wt%, and particle size distribution: 1 wt% fine powder above a 160-mesh sieve and 55 wt% fine powder below a 320-mesh sieve.

[0171] Comparative Example 8

[0172] Compared with Example 3, the mass ratio of microcrystalline graphite and T395 graphite powder in Comparative Example 8 is 4:1.5. The material list of Comparative Example 8 is shown in Table 11.

[0173] Table 11

[0174]

[0175] Preparation method:

[0176] S1. Dry mix coke powder, graphite and carbon black at 110℃ for 60 minutes, add modified asphalt, and close mix at 170℃ for 90 minutes to obtain a paste. Roll the paste at 170℃ to obtain a 3mm thick sheet.

[0177] S2. Grind the rolled sheet obtained in step S1 into powder, stir and mix evenly to obtain fine powder;

[0178] S3. Pour the fine powder obtained in step S2 into a mold and press it to obtain the coarse product;

[0179] S4. Roast the crude product obtained in step S3.

[0180] S5. Remove from the oven after cooling.

[0181] The roasting curve is as follows: the temperature is increased from room temperature to 280℃ at 50℃ / h, then increased to 500℃ at 1℃ / h, then increased to 750℃ at 2.5℃ / h, then increased to 900℃ at 5℃ / h, then increased to 1200℃ at 10℃ / h, and then held at 1200℃ for 68 hours before the furnace is shut down.

[0182] The fine powder obtained in step S2 has the following characteristics: moisture content of 0.2 wt%, volatile matter of 12 wt%, and particle size distribution: 1 wt% fine powder above a 160-mesh sieve and 55 wt% fine powder below a 320-mesh sieve.

[0183] Comparative Example 9

[0184] Compared with Example 3, the fine powder prepared in step S2 of Comparative Example 9 has the following characteristics: moisture content of 3 wt%, volatile matter of 20 wt%, and particle size distribution of 10 wt% above a 160-mesh sieve and 40 wt% below a 320-mesh sieve. The material list for Comparative Example 9 is shown in Table 12.

[0185] Table 12

[0186]

[0187] Preparation method:

[0188] S1. Dry mix coke powder, graphite and carbon black at 110℃ for 60 minutes, add modified asphalt, and close mix at 170℃ for 90 minutes to obtain a paste. Roll the paste at 170℃ to obtain a 3mm thick sheet.

[0189] S2. Grind the rolled sheet obtained in step S1 into powder, stir and mix evenly to obtain fine powder;

[0190] S3. Pour the fine powder obtained in step S2 into a mold and press it to obtain the coarse product;

[0191] S4. Roast the crude product obtained in step S3.

[0192] S5. Remove from the oven after cooling.

[0193] The roasting curve is as follows: the temperature is increased from room temperature to 280℃ at 50℃ / h, then increased to 500℃ at 5℃ / h, then increased to 750℃ at 2℃ / h, then increased to 900℃ at 4℃ / h, then increased to 1200℃ at 10℃ / h, and then the furnace is stopped after holding at 1200℃ for 68 hours.

[0194] The fine powder obtained in step S2 has the following characteristics: moisture content of 3 wt%, volatile matter of 20 wt%, and particle size distribution: 10 wt% fine powder above 160 mesh and 40 wt% fine powder below 320 mesh.

[0195] Comparative Example 10

[0196] Compared to Example 1 in CN106672959A, it only underwent one calcination.

[0197] The raw materials used in Example 1 of CN106672959A were coke powder, microcrystalline graphite, and coal tar pitch powder in a mass ratio of 40:30:30.

[0198] The coke powder is made by mixing delayed petroleum coke powder (average particle size 90-250μm) and coal tar at a mass ratio of 80:20 at 150℃ for 45 minutes, cooling, then crushing into 250-300μm particles, cold isostatic pressing, and grinding into 5-10μm coke powder.

[0199] The three components, coke powder, microcrystalline graphite (5-10μm) and coal tar pitch powder, are mixed at 160-200℃ according to the required proportions. The mixed material is then ground and pressed according to conventional processes, and subjected to calcination heat treatment at 950-1150℃ for 360-420 hours.

[0200] II. Performance Testing

[0201] 1. The density, open porosity, flexural strength, compressive strength and Shore hardness of the carbonaceous materials prepared in Examples 1-3 and Comparative Examples 1-10 were measured, and the results are shown in Table 13.

[0202] The density test method was conducted according to "Physical and Chemical Test Methods for Electro-Carbonized Products Part 14: Bulk Density" (JB / T8133.14-2013); the open porosity test method was conducted according to GB / T 24529-2009 "Determination of Apparent Porosity of Carbon Materials"; the flexural strength test method was conducted according to "Physical and Chemical Test Methods for Electro-Carbonized Products Part 7: Flexural Strength" (JB / T8133.7-2013); the compressive strength test method was conducted according to "Physical and Chemical Test Methods for Electro-Carbonized Products Part 8: Compressive Strength" (JB / T8133.8-2013); and the Shore hardness test method was conducted according to "Physical and Chemical Test Methods for Electro-Carbonized Products Part 4: Shore Hardness".

[0203] (JB / T8133.4-2013) is being implemented.

[0204] Table 13

[0205]

[0206] The technical solutions claimed in this invention, embodiments 1-3, have a density of 1.64-1.67 g / cm³. 3 It has an open porosity of 7.9-9.6%, a flexural strength of 58-67 MPa, a compressive strength of 83-89 MPa, and a Shore hardness of 76-80.

[0207] Compared with Example 3, the change in the percentage of raw material mass in Comparative Example 1 is not within the scope of protection of this application, and its density is 1.58 g / cm³. 3 The porosity is 15%, the flexural strength is 31-32 MPa, the compressive strength is 123 MPa, and the Shore hardness is 62-66. The carbonaceous materials made from it have reduced performance.

[0208] Compared with Example 3, the changes in the relationship between the volatile matter content and dosage of coke powder in Comparative Examples 2 and 7 are not within the scope of protection of this application, and their densities are 1.54-1.57 g / cm³. 3 The porosity is 17-18%, the flexural strength is 31-32 MPa, the compressive strength is 83-89 MPa, and the Shore hardness is 57-66. The properties of the carbonaceous materials made from it are reduced.

[0209] Compared with Example 3, the changes in the type and amount of graphite in Comparative Examples 3-5 and Comparative Example 8 are not within the scope of protection of this application, and their densities are 1.59-1.62 g / cm³. 3 The porosity is 11-15%, the flexural strength is 35-51 MPa, the compressive strength is 116-137 MPa, and the Shore hardness is 65-85. The carbonaceous materials made from it have reduced performance.

[0210] Compared to Example 3, Comparative Example 6, which changed the type of carbon black, is not within the scope of protection of this application; its density is 1.60 g / cm³.3 The porosity is 13%, the flexural strength is 44 MPa, the compressive strength is 127 MPa, and the Shore hardness is 86. The performance of the carbonaceous material produced by it is reduced.

[0211] Compared with Example 3, the change in the fine powder parameters of step S2 in Comparative Example 9 is not within the scope of protection of this application; its density is 1.56 g / cm³. 3 The porosity is 14%, the flexural strength is 43 MPa, the compressive strength is 121 MPa, and the Shore hardness is 68. The performance of the carbonaceous material produced by it is reduced.

[0212] Compared to Example 3, Comparative Example 10 is a prior art product, which undergoes only one calcination and has a density of 1.53 g / cm³. 3 The porosity is 19%, the flexural strength is 36 MPa, the compressive strength is 103 MPa, and the Shore hardness is 60. The performance of the carbonaceous material produced by it is reduced.

[0213] 2. Impregnate the carbonaceous materials obtained in Examples 1-3 and Comparative Examples 1-10 with metallic antimony to prepare carbonaceous sealing materials. The amount of impregnating metal required to pass the bulk density test of the carbonaceous sealing materials obtained in Examples 1-3 and Comparative Examples 1-10 is shown in Table 14.

[0214] Table 14

[0215]

[0216]

[0217] The amount of impregnating metal added in Examples 1-3 of this invention is small: 0.461-0.575 g / cm³. 3 This saves costs.

[0218] Compared with Example 3, the change in the percentage of raw material mass in Comparative Example 1 is not within the scope of protection of this application, and its impregnation metal addition amount is 0.935 g / cm³. 3 This increases costs.

[0219] Compared with Example 3, the changes in the relationship between the volatile matter content and dosage of coke powder in Comparative Examples 2 and 7 are not within the scope of protection of this application, as their impregnation metal addition amount is greater than 1.069 g / cm³. 3 This increases costs.

[0220] Compared with Example 3, the changes in the type and amount of graphite in Comparative Examples 3-5 and Comparative Example 8 are not within the scope of protection of this application, and their impregnation metal addition amount is 0.668-0.935 g / cm³. 3 This increases costs.

[0221] Compared to Example 3, Comparative Example 6, which changed the type of carbon black, is not within the scope of protection of this application, and its impregnation metal addition amount is 0.802 g / cm³. 3 This increases costs.

[0222] Compared with Example 3, the change in the fine powder parameters of step S2 in Comparative Example 9 is not within the scope of protection of this application, and its impregnation metal addition amount is 0.868 g / cm³. 3 This increases costs.

[0223] Comparative Example 10 is a prior art example, which involves only one firing and has an impregnation metal addition of 1.202 g / cm³. 3 This increases costs.

[0224] Finally, it should be noted that the above content is only used to illustrate the technical solution of the present invention, and is not intended to limit the scope of protection of the present invention. Simple modifications or equivalent substitutions made by those skilled in the art to the technical solution of the present invention do not depart from the essence and scope of the technical solution of the present invention.

Claims

1. A carbonaceous material, characterized in that, 30-45% coke powder, 25-30% graphite, 3.5-8% carbon black and 26.5-33% pitch by mass percentage; the coke powder is composed of coke powder containing 1-2% volatile matter and coke powder containing 8-14% volatile matter; the graphite is microcrystalline graphite and T395 graphite powder; the pitch is modified pitch containing 45-60% volatile matter; the mass ratio of the coke powder containing 1-2% volatile matter and the coke powder containing 8-14% volatile matter is 1.5-2.5:0.8-1; the mass ratio of the microcrystalline graphite and the T395 graphite powder is 4-5:0.5-1; the preparation method of the carbonaceous material comprises the following steps: S1, dry mixing the coke powder, graphite and carbon black, adding modified pitch, closed mixing to obtain paste, rolling the paste to obtain rolled sheet; S2, grinding the rolled sheet obtained in step S1, stirring and mixing uniformly to obtain fine powder; S3, pouring the fine powder obtained in step S2 into a mold to press to obtain crude product; S4, roasting the crude product obtained in step S3; S5, taking out after cooling; the moisture content of the fine powder in step S2 is 0-1wt%, the volatile matter content is 12-18wt%, and the screening particle size is that the content of fine powder above 160 mesh screen is 0-5wt% and the content of fine powder below 320 mesh screen is 55-60wt%; the dry mixing condition in step S1 is 110-130℃ dry mixing for 60-90min; the closed mixing condition in step S1 is 170-180℃ closed mixing for 90min.

2. The carbonaceous material according to claim 1, characterized in that, the carbon black is N330 carbon black.

3. The carbonaceous material according to claim 1, characterized in that, the coke powder containing 1-2% volatile matter has a 320 mesh screen passing rate of 80-90%.

4. The carbonaceous material of claim 1, wherein, the coke powder containing 8-14% volatile matter has a particle size of D50: 5-10μm.

5. The carbonaceous material of claim 1, wherein, the microcrystalline graphite has a 320 mesh screen passing rate of 80-85%.

6. The carbonaceous material of claim 1, wherein, the T395 graphite powder has a 320 mesh screen passing rate of 75-85%.

7. The carbonaceous material of claim 1, wherein, the T395 graphite powder has a PH value of 7.

8. The preparation method of the carbonaceous material according to any one of claims 1-7, comprising the following steps: S1, dry mixing the coke powder, graphite and carbon black, adding modified pitch, closed mixing to obtain paste, rolling the paste to obtain rolled sheet; S2, grinding the rolled sheet obtained in step S1, stirring and mixing uniformly to obtain fine powder; S3, pouring the fine powder obtained in step S2 into a mold to press to obtain crude product; S4, roasting the crude product obtained in step S3; S5, taking out after cooling; the moisture content of the fine powder in step S2 is 0-1wt%, the volatile matter content is 12-18wt%, and the screening particle size is that the content of fine powder above 160 mesh screen is 0-5wt% and the content of fine powder below 320 mesh screen is 55-60wt%.

9. The production method according to claim 8, characterized by, the rolling temperature in step S1 is 170-200℃.

10. The preparation method according to claim 8, characterized in that, the thickness of the rolled sheet in step S1 is 2-4mm.

11. The preparation method according to claim 8, characterized in that, The roasting conditions of step S4 are: from room temperature to 250-280°C at 45-50°C / h, to 450-500°C at 1-2°C / h, to 700-750°C at 2-3°C / h, to 850-900°C at 4-5°C / h, to 1100-1200°C at 5-10°C / h, and holding at 1100-1200°C for 60-70h before stopping the furnace.

12. A carbonaceous sealing material, characterized by, A carbonaceous material according to any one of claims 1 to 7 or a carbonaceous material produced by the method according to any one of claims 8 to 11.

13. A bearing, characterized by A carbonaceous material according to any one of claims 1 to 7 or a carbonaceous material produced by the method according to any one of claims 8 to 11.

14. An apparatus, comprising: A carbonaceous sealing material according to claim 12 and / or a bearing according to claim 13.

Citation Information

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