Method for the continuous synthesis of cobalt disulfide powder at high temperature by solid phase

Abstract

The application discloses a method for continuously synthesizing cobalt disulfide powder in a high-temperature solid phase, and belongs to the technical field of functional material preparation. The method comprises the following steps: uniformly mixing high-purity cobalt powder and high-purity sulfur powder, loading the mixture into a boat, pushing the boat into a full-automatic boat pushing furnace production line, setting the interval temperature of the boat pushing furnace and the sulfuration time, and synthesizing high-purity cobalt disulfide through multiple sulfurations. The cobalt disulfide synthesized by the method has high purity and low impurity content, and the battery made of the cobalt disulfide has the characteristics of long discharge time, good thermal stability and good chemical stability. The boat pushing furnace production line can realize full-automatic continuous production, has high efficiency, and can recycle the excess sulfur in the production process with pure nitrogen in the production line, so that the cost is low, and the problem that the existing synthesis technology of cobalt disulfide cannot meet the demand of industrial large-scale production can be effectively solved.

Description

Technical Field

[0001] This invention belongs to the field of functional material preparation technology, and relates to a method for preparing cobalt disulfide, specifically a method for high-temperature solid-phase continuous synthesis of cobalt disulfide powder. Background Technology

[0002] Thermal batteries are thermally activated storage batteries. At room temperature, the electrolyte is solid. During use, the electrolyte melts into an ionic conductor under the action of its own heating system, and then the battery begins to discharge. With the rapid development of technology, lithium-based thermal batteries using iron disulfide as the positive electrode material are no longer sufficient to meet the performance requirements of thermal batteries. Cobalt dioxide has similar properties to iron disulfide, and also possesses advantages that iron disulfide lacks, such as good conductivity, low self-discharge rate, and high operating voltage. Cobalt disulfide is an important positive electrode material in the preparation of high-power thermal batteries. Its application can effectively solve problems such as overpressure, narrow voltage range, short operating time, and performance degradation during long-term storage in cobalt disulfide system thermal batteries.

[0003] Cobalt disulfide is typically produced from sulfur powder and cobalt powder using high-temperature heating. The preparation process involves weighing and mixing metallic cobalt powder and sulfur powder in a specific ratio, then sealing the mixture in a quartz tube. After this process, the sealed quartz tube is gently placed in a stainless steel reactor for heating. After the reaction, cobalt disulfide crystals are obtained through natural cooling. These crystals are then pulverized and screened. Finally, high-temperature desulfurization and lithiation peak reduction yield cobalt disulfide suitable for use in high-power thermal batteries.

[0004] CN1594108A discloses a method for synthesizing high-purity cobalt disulfide powder under atmospheric pressure. The method involves uniformly mixing high-purity elemental cobalt powder and sulfur powder, placing the mixture in a high-temperature resistant container, degassing the system under vacuum, and then placing it in a muffle furnace with a temperature gradient under an inert atmosphere such as argon or nitrogen. The sulfur is separated from the product at atmospheric pressure within a range of 100-700℃, and the mixture is cooled to obtain a crude product. The crude product is then ground, sieved, or classified, and the sulfur is again separated from the product under an inert atmosphere such as argon or nitrogen within a range of 100-700℃, followed by cooling to obtain high-purity cobalt disulfide powder with a purity greater than 99%. This method uses atmospheric pressure production and processes each furnace individually, resulting in a long production process, making continuous production impossible and costly, which is not conducive to large-scale industrial application. Furthermore, while the method claims a purity greater than 99%, it does not perform crystal form testing or thermogravimetric analysis, therefore it cannot prove whether the claimed purity of the final product refers to the purity of S or Co, or the purity of CoS2.

[0005] Therefore, there is an urgent need to study a low-cost, high-efficiency method for synthesizing cobalt disulfide that is suitable for large-scale industrial production. Summary of the Invention

[0006] The technical problem to be solved by this invention is that existing technologies for synthesizing cobalt disulfide cannot meet the needs of large-scale industrial production.

[0007] The technical solution adopted by this invention to solve its technical problem is: a method for high-temperature solid-phase continuous synthesis of cobalt disulfide powder: high-purity cobalt powder and high-purity sulfur powder are mixed evenly and then loaded into a boat, which is pushed into a fully automatic boat-pushing furnace production line. By setting the temperature range and sulfidation time of the boat-pushing furnace, high-purity cobalt disulfide is synthesized through multiple sulfidation processes; the fully automatic boat-pushing furnace production line includes a feeding zone, a synthesis zone, a cooling zone, and a discharging zone.

[0008] The synthesis zone is divided into seven temperature zones: Zone 1 is vulcanized at 100-110℃ for 1-2 hours, Zone 2 at 160-220℃ for 1-2 hours, Zone 3 at 300-350℃ for 2-4 hours, Zones 4 to 6 at 400-440℃ for 2-4 hours, and Zone 7 at 540-600℃ for 2-4 hours.

[0009] Furthermore, in Zone 1, the vulcanization time is 1.4-1.6 hours at 100-110℃; in Zone 2, it is 1.4-1.6 hours at 190-200℃; in Zone 3, it is 2.9-3.1 hours at 320-330℃; in Zones 4-6, it is 2.9-3.1 hours at 410-430℃; and in Zone 7, it is 2.9-3.1 hours at 560-580℃.

[0010] The cooling zone includes a slow cooling zone and a water cooling zone. The temperature is cooled to ≤100°C in the slow cooling zone and to near room temperature in the water cooling zone.

[0011] The above production process is carried out under a fully sealed pure nitrogen atmosphere with a purity of ≥99.99%, and the flow rate of pure nitrogen introduced into the fully automated pusher furnace production line is 15-25 Nm³. 3 / h, maintaining a slight positive pressure within the fully automated pushboat furnace production line.

[0012] Furthermore, the micro-positive pressure refers to the air pressure inside the fully automated pushboat furnace production line being 20-50 Pa higher than the external atmospheric pressure.

[0013] Among them, the purity of the above-mentioned high-purity cobalt disulfide is ≥99%, the thermal stability is no decomposition and weight loss at 620℃, and the weight loss rate is ≤5% at 700℃.

[0014] A method for continuous high-temperature solid-phase synthesis of cobalt disulfide powder specifically includes the following steps:

[0015] a. Mix high-purity cobalt powder and high-purity sulfur powder at a mass ratio of 1:1-1.5 and load them into a boat. Then, put the boat into a fully automatic push-boat furnace production line for sulfidation. After discharge, deagglomerate, crush and classify the material until it passes through an 80-mesh sieve to obtain semi-finished product 1.

[0016] b. Mix semi-finished product 1 and high-purity sulfur powder at a mass ratio of 1:1-1.5, load them into a boat, then perform sulfidation, and after discharge, pass them through an 80-mesh sieve to obtain semi-finished product 2;

[0017] c. Mix semi-finished product 2 and high-purity sulfur powder at a mass ratio of 1:0.7-1, load the mixture into a boat, and then perform sulfidation. After discharge, pass the mixture through an 80-mesh sieve to obtain semi-finished product 3.

[0018] d. Mix semi-finished product 3 and high-purity sulfur powder at a mass ratio of 1:0.5-0.7, load them into a boat, and then perform sulfidation. After discharge, pass through a 60-mesh sieve. After passing the test according to the internal control standard requirements, mix the batches together, and then package and label them to obtain high-purity cobalt disulfide products.

[0019] Furthermore, in the above-mentioned method for continuous synthesis of cobalt disulfide powder in a high-temperature solid phase, all processes are carried out in a dry environment with an ambient humidity of ≤2%.

[0020] Furthermore, during the loading of the boat, the amount of boat material in step a is controlled to be 6-7 kg, and the amount of boat material in steps b, c, and d is controlled to be 8-12 kg.

[0021] Furthermore, during the vulcanization process in steps a, b, c, and d above, the rate at which the boat enters the fully automated boat-pushing furnace production line is controlled to be 1-2 hours per boat.

[0022] Furthermore, in step a above, the total cobalt content in the semi-finished product 1 is ≤58%.

[0023] Furthermore, in step b above, the total cobalt content in the semi-finished product 2 is ≤52%.

[0024] Furthermore, in step c above, the total cobalt content in the semi-finished product 3 is ≤50%.

[0025] Furthermore, in step d above, the internal control standard requires that the cobalt disulfide content be ≥99%, the total cobalt content be 47.4-48.7%, the total sulfur content be 51.5-52.7%, and the elemental sulfur content be ≤0.2%.

[0026] Furthermore, the above-mentioned method for continuous high-temperature solid-phase synthesis of cobalt disulfide powder is equipped with a sulfur recovery device. After each sulfidation is completed, the excess sulfur powder is vaporized at high temperature for 3 hours and then carried into the sulfur recovery device for collection along with pure nitrogen.

[0027] The beneficial effects of this invention are as follows: the CoS2 synthesized using the high-temperature solid-phase continuous synthesis method of cobalt disulfide powder provided by this invention has high purity (≥99%) and low impurity content; batteries made from it exhibit long discharge time, good thermal stability, and good chemical stability. Compared with traditional methods for preparing cobalt disulfide, the push-boat furnace production line of this invention can automatically and continuously synthesize cobalt disulfide, overcoming the shortcomings of traditional single-furnace process control instability, long production time, and low output. The high-temperature solid-phase continuous synthesis method of cobalt disulfide powder of this invention has high output and high efficiency. Excess sulfur during the production process can be recovered and reused along with pure nitrogen in the production line, resulting in low cost. It can meet the needs of large-scale industrial production and has promotional application value. Attached Figure Description

[0028] Figure 1 This is a schematic diagram of the zoning layout of the fully automated push-boat furnace production line of the present invention;

[0029] Figure 2 This is a physical image of the fully automated pushboat furnace production line of the present invention;

[0030] Figure 3 This is a flowchart of the production process of the present invention;

[0031] Figure 4 Thermogravimetric analysis curve of Example 1 of the present invention;

[0032] Figure 5 This is a phase analysis diagram of Example 1 of the present invention;

[0033] Figure 6 This is an electron microscope image of Embodiment 1 of the present invention. Detailed Implementation

[0034] The technical solution of the present invention can be implemented in the following manner.

[0035] A method for high-temperature solid-phase continuous synthesis of cobalt disulfide powder: High-purity cobalt powder and high-purity sulfur powder are mixed evenly in a certain proportion, loaded into a boat in a dry environment, and pushed into a fully automatic boat-pushing furnace production line. By setting different temperature zones and sulfidation times in the boat-pushing furnace, high-purity cobalt disulfide is synthesized through multiple sulfidation processes.

[0036] Preferably, the above-mentioned high-purity cobalt powder must meet the following quality requirements: (1) Appearance: black powder, free from lumps and visible impurities; (2) Chemical indicators: total cobalt ≥ 99.50%, iron ≤ 0.05%, nickel ≤ 0.05%, silicon ≤ 0.02%.

[0037] Preferably, the above-mentioned high-purity sulfur powder must meet the following quality requirements: (1) Appearance: light yellow powder, free from lumps and visible impurities; (2) Chemical indicators: total sulfur (TS) ≥ 99.50%, moisture ≤ 2.00%, ash ≤ 0.10%, organic matter content ≤ 0.30%.

[0038] The zonal layout of the fully automated pushboat furnace production line described in this invention is as follows: Figure 1 , 2 As shown, the fully automated push-boat furnace production line includes a feeding zone, a synthesis zone, a cooling zone, and a discharging zone. The synthesis zone is divided into seven temperature zones, and the cooling zone is divided into a slow cooling zone, a water-cooled zone 1, and a water-cooled zone 2.

[0039] Preferably, the synthesis zone is controlled as follows: Zone 1 is vulcanized at 100-110℃ for 1-2 hours, Zone 2 at 160-220℃ for 1-2 hours, Zone 3 at 300-350℃ for 2-4 hours, Zones 4 to 6 at 400-440℃ for 2-4 hours respectively, and Zone 7 at 540-600℃ for 2-4 hours.

[0040] More preferably, the vulcanization reaction in the synthesis zone is controlled as follows: Zone 1 is vulcanized at 100-110℃ for 1.4-1.6h; Zone 2 is vulcanized at 190-200℃ for 1.4-1.6h; Zone 3 is vulcanized at 320-330℃ for 2.9-3.1h; Zones 4 to 6 are vulcanized at 410-430℃ for 2.9-3.1h respectively; and Zone 7 is vulcanized at 560-580℃ for 2.9-3.1h.

[0041] When the boat enters the fully automated push-boat furnace production line and reaches synthesis zone one, the surface water of the material can be removed. When the boat passes through synthesis zones two and three, the sulfur powder in the material begins to melt, and the liquid sulfur can fully coat Co to ensure that the subsequent sulfidation reaction proceeds fully. It enters zones four, five and six to start sulfidation to generate CoS2. Finally, it passes through zone seven for gasification. After sulfidation, the excess S is gasified at high temperature and carried into the sulfur recovery device for collection along with pure nitrogen.

[0042] Preferably, the vessel is cooled to ≤100°C in a slow cooling zone, then cooled to near room temperature in a water cooling zone, and then enters the discharge zone.

[0043] Figure 1 "Air cooling" refers to a situation where, due to the design of equipment in actual production lines, it is impossible for the boat / dish to seamlessly connect directly from the slow cooling zone to the first water cooling zone and from the first water cooling zone to the second water cooling zone. Instead, after exiting the slow cooling zone, the boat / dish passes through a short gap before entering the first water cooling zone. In this invention, this gap is considered air cooling. The same principle applies when moving from the first water cooling zone to the second water cooling zone. The air cooling process in this invention does not affect the overall process control.

[0044] Preferably, the boat is loaded using a corundum boat or a ceramic boat. After loading, the boat is pushed into the feeding zone of the fully automated boat-pushing furnace production line. Pure nitrogen gas is introduced into the fully automated boat-pushing furnace production line from the water-cooled secondary zone and is discharged along with sulfur vapor after the feeding zone and before the synthesis zone. The production process is carried out under a fully sealed pure nitrogen atmosphere, with a pure nitrogen purity ≥ 99.99%, and the flow rate of pure nitrogen introduced into the fully automated boat-pushing furnace production line is 15-25 Nm³.3 / h, maintaining a slight positive pressure within the fully automated pushboat furnace production line.

[0045] Preferably, the micro-positive pressure refers to the gas pressure inside the fully automatic push-boat furnace production line being 20-50 Pa higher than the external atmospheric pressure. The purpose of maintaining a micro-positive pressure inside the fully automatic push-boat furnace production line is to ensure that there is pressure inside the production line, which can prevent external gases or impurities from entering, and ensure that the gas or substances inside the push-boat furnace can only be output from the inside to the outside, thereby ensuring that there are no impurities intruding during the production process and improving the purity of the product.

[0046] Preferably, the high-purity cobalt disulfide has a purity of ≥99%, thermal stability of no decomposition and weight loss at 620℃, and a weight loss rate of ≤5% at 700℃.

[0047] The process flow of the above-mentioned high-temperature solid-phase continuous synthesis of cobalt disulfide powder is as follows: Figure 3 As shown, the specific steps include the following:

[0048] a. Mix high-purity cobalt powder and high-purity sulfur powder at a mass ratio of 1:1-1.5 and load them into a boat. Then, put the boat into a fully automatic push-boat furnace production line for sulfidation. After discharge, deagglomerate, crush and classify the material until it passes through an 80-mesh sieve to obtain semi-finished product 1.

[0049] b. Mix semi-finished product 1 and high-purity sulfur powder at a mass ratio of 1:1-1.5, load them into a boat, then perform sulfidation, and after discharge, pass them through an 80-mesh sieve to obtain semi-finished product 2;

[0050] c. Mix semi-finished product 2 and high-purity sulfur powder at a mass ratio of 1:0.7-1, load the mixture into a boat, and then perform sulfidation. After discharge, pass the mixture through an 80-mesh sieve to obtain semi-finished product 3.

[0051] d. Mix semi-finished product 3 and high-purity sulfur powder at a mass ratio of 1:0.5-0.7, load them into a boat, and then perform sulfidation. After discharge, pass through a 60-mesh sieve. After passing the test according to the internal control standard requirements, mix the batches together, and then package and label them to obtain high-purity cobalt disulfide products.

[0052] Preferably, the mixing is carried out using a mixing tank. Before adding materials, the mixing tank is purged with pure nitrogen. After adding materials, pure nitrogen is introduced again for 2-3 minutes to ensure positive pressure inside the tank. The amount of materials added to the mixing tank each time is less than 2 / 3 of the volume of the mixing tank.

[0053] More preferably, during the mixing in steps a, b, and c above, the mixing time is ≥1 hour for both forward and reverse mixing in the mixing tank, until the color of the mixed material is consistent or the total cobalt content measured by sampling deviates from the theoretically calculated cobalt content by less than 0.50%; during the batch mixing in step d, the mixing time is ≥2 hours for both forward and reverse mixing in the mixing tank, until the color of the mixed material is consistent.

[0054] Preferably, during the loading of the boat, the amount of boat material in step a is controlled to be 6-7 kg, and the amount of boat material in steps b, c, and d is controlled to be 8-12 kg.

[0055] Preferably, when controlling the vulcanization process in steps a, b, c, and d above, the rate at which the boat enters the fully automatic boat-pushing furnace production line is controlled to be 1-2 hours per boat.

[0056] Preferably, in step a above, the total cobalt content in the semi-finished product 1 is ≤58%.

[0057] Preferably, in step b above, the total cobalt content in the semi-finished product 2 is ≤52%.

[0058] Preferably, in step c above, the total cobalt content in the semi-finished product 3 is ≤50%.

[0059] Preferably, in step d above, the internal control standard requires that the cobalt disulfide content be ≥99%, the total cobalt content be 47.4-48.7%, the total sulfur content be 51.5-52.7%, and the elemental sulfur content be ≤0.2%.

[0060] Preferably, the above-mentioned method for continuous high-temperature solid-phase synthesis of cobalt disulfide powder is equipped with a sulfur recovery device. After each sulfidation is completed, the excess sulfur powder is vaporized at high temperature for 3 hours and then carried into the sulfur recovery device for collection along with pure nitrogen.

[0061] The high-temperature solid-phase continuous synthesis method for cobalt disulfide powder of this invention is carried out entirely in a dry environment with an ambient humidity of ≤2%. After each sulfidation, if there is any material remaining on the sieve, it must be deagglomerated, crushed, and graded until all material passes through the sieve. In step d, if any unqualified products are found during testing according to internal control standards, they are returned to step d as semi-finished product 3 for further sulfidation until all products are qualified. In actual production, the qualified products are batch-mixed, packaged, and labeled to obtain the high-purity cobalt disulfide product.

[0062] The technical solution and effects of the present invention will be further explained below through practical examples.

[0063] Example

[0064] This invention provides two sets of examples 1-2 of preparing high-purity cobalt disulfide powder using the above-mentioned high-temperature solid-phase continuous synthesis method for cobalt disulfide powder. The specific experimental steps are as follows.

[0065] I. Raw Material Preparation

[0066] High-purity cobalt powder (TCo≥99.50%) and purchased high-purity sulfur powder (TS≥99.50%) were used. The sulfur powder conformed to the national standard GB / T2449.1-2021. The specific monitoring indicators and results of the raw materials are shown in Table 1.

[0067] Table 1 Raw Material Testing Table

[0068]

[0069] II. Experimental Procedure

[0070] Cobalt disulfide powder was prepared according to the process flow of high-temperature solid-phase continuous synthesis, and the process control parameters are as follows.

[0071] 1. Process control parameters of the fully automatic pusher furnace production line: (1) Temperature zone control (as shown in Table 2); (2) Pushing frequency: one pusher every 1-2 hours; (3) Nitrogen flow rate: 15-25 Nm 3 / h (pure nitrogen); (4) uniform mixing and smooth fabric distribution; (5) spray device frequency: 20-40Hz.

[0072] Table 2 Temperature Zone Control of Pushboat Furnace

[0073] Temperature setting ℃ 100-110 190-200 320-330 410-430 410-430 410-430 560-580 Reaction time / h 1.5 1.5 3 3 3 3 3

[0074] 2. Depolymerization and classification process control parameters: (1) Nitrogen protection: purity ≥ 99.99%; (2) Main unit frequency: 10-30Hz; (3) Feeding frequency: 10-40Hz.

[0075] 3. Screening process control parameters: (1) Semi-finished products pass through an 80-mesh sieve (pure nitrogen as protective gas, ultrasonic vibration screening); (2) Finished products pass through a 60-mesh sieve (pure nitrogen as protective gas, ultrasonic vibration screening).

[0076] 4. Mixing process control parameters: (1) Motor frequency: 25Hz; (2) Forward and reverse rotation: 2-3h each; (3) Feeding amount: ≤3 tons.

[0077] III. Finished Product Inspection

[0078] High-purity cobalt disulfide was prepared according to the above process flow and parameters, and then tested. The test results are shown in Table 3 (purity was calculated based on the theoretical Co or S content in CoS2). The thermogravimetric analysis curves are shown in Table 3. Figure 4 As shown, the phase analysis diagram is as follows: Figure 5 As shown in Figure 6, the electron microscope morphology image shows that the main phase of the product prepared in this embodiment is CoS2, and it does not contain other impurities.

[0079] Table 3. Synthetic CoS2 Detection Report

[0080]

[0081]

[0082] The production process of this invention includes four inspection points: raw material inspection, furnace charge inspection, depolymerization and screening mixing inspection, and finished product inspection. According to internal control standards, except for the finished product which undergoes initial and re-inspections, all other inspection points are implemented for every boat. Through the reasonable setup of inspection points and the appropriate number of inspections, product quality can be effectively controlled. No defective products are produced during the production process. Substandard semi-finished products will undergo a second vulcanization process to meet the required technical specifications.

[0083] In production, a fully automatic push-boat furnace production line of this invention can produce 100-120 kg of semi-finished products per day through the first vulcanization, 80-120 kg of semi-finished products per day through the second vulcanization, 100-140 kg of finished products per day through the third vulcanization, and 140-160 kg of finished products per day through the fourth vulcanization. The product yield is ≥90%, and the monthly output is 1.5-2 tons, which has high economic value.

[0084] The cobalt disulfide product of this invention employs a unique high-temperature solid-phase thermal synthesis technology and process, with the entire process conducted under pure nitrogen protection to ensure stable quality. The production line, site layout, and production environment of the cobalt disulfide product meet the process requirements. The incoming inspection and supply capacity of raw materials (cobalt powder and sulfur) can guarantee the needs of mass production. Inspection points are rationally set up during the product manufacturing process, ensuring effective control. The produced cobalt disulfide product has passed the company's inspection and meets the technical requirements.

Claims

1. A method for continuous high-temperature solid-phase synthesis of cobalt disulfide powder, characterized in that: High-purity cobalt powder and high-purity sulfur powder are mixed evenly and then loaded into a boat. The boat is then pushed into a fully automatic push-boat furnace production line. By setting the temperature range and sulfidation time of the push-boat furnace, high-purity cobalt disulfide is synthesized through multiple sulfidation processes. The fully automatic push-boat furnace production line includes a feeding zone, a synthesis zone, a cooling zone, and a discharging zone. The synthesis zone is divided into seven temperature zones: Zone 1 is vulcanized at 100-110℃ for 1-2 hours, Zone 2 at 160-220℃ for 1-2 hours, Zone 3 at 300-350℃ for 2-4 hours, Zones 4 to 6 at 400-440℃ for 2-4 hours, and Zone 7 at 540-600℃ for 2-4 hours. Specifically, the steps include the following: a. Mix high-purity cobalt powder and high-purity sulfur powder at a mass ratio of 1:1-1.5 and load them into a boat. Then, put the boat into a fully automatic push-boat furnace production line for sulfidation. After discharge, deagglomerate, crush and classify the material until it passes through an 80-mesh sieve to obtain semi-finished product 1. b. Mix semi-finished product 1 and high-purity sulfur powder at a mass ratio of 1:1-1.5, load them into a boat, then perform sulfidation, and after discharge, pass them through an 80-mesh sieve to obtain semi-finished product 2; c. Mix semi-finished product 2 and high-purity sulfur powder at a mass ratio of 1:0.7-1, load the mixture into a boat, and then perform sulfidation. After discharge, pass the mixture through an 80-mesh sieve to obtain semi-finished product 3. d. Mix semi-finished product 3 and high-purity sulfur powder at a mass ratio of 1:0.5-0.7, load them into a boat, and then carry out sulfidation. After discharge, pass through a 60-mesh sieve. After passing the test according to the internal control standard requirements, mix the batches together, and then package and label them to obtain high-purity cobalt disulfide products. In step d, the internal control standard requires that the cobalt disulfide content be ≥99%, the total cobalt content be 47.4-48.7%, the total sulfur content be 51.5-52.7%, and the elemental sulfur content be ≤0.2%.

2. The method for continuous high-temperature solid-phase synthesis of cobalt disulfide powder according to claim 1, characterized in that: Zone 1 is vulcanized at 100-110℃ for 1.4-1.6 hours, Zone 2 at 190-200℃ for 1.4-1.6 hours, Zone 3 at 320-330℃ for 2.9-3.1 hours, Zones 4-6 at 410-430℃ for 2.9-3.1 hours, and Zone 7 at 560-580℃ for 2.9-3.1 hours.

3. The method for continuous high-temperature solid-phase synthesis of cobalt disulfide powder according to claim 1, characterized in that: The cooling zone includes a slow cooling zone and a water cooling zone. The temperature is cooled to ≤100°C in the slow cooling zone and to near room temperature in the water cooling zone.

4. The method for continuous high-temperature solid-phase synthesis of cobalt disulfide powder according to claim 1, characterized in that: The production process is carried out under a fully sealed pure nitrogen atmosphere with a purity of ≥99.99%. The flow rate of pure nitrogen introduced into the fully automated pusher furnace production line is 15-25 Nm³. 3 / h, maintaining a slight positive pressure within the fully automated pushboat furnace production line.

5. The method for continuous high-temperature solid-phase synthesis of cobalt disulfide powder according to claim 1, characterized in that: The high-purity cobalt disulfide has a purity of ≥99%, thermal stability of no decomposition or weight loss at 620℃, and a weight loss rate of ≤5% at 700℃.

6. The method for continuous high-temperature solid-phase synthesis of cobalt disulfide powder according to claim 1, characterized in that: When loading the boat, control the amount of boat material in step a to be 6-7 kg, and the amount of boat material in steps b, c, and d to be 8-12 kg; when vulcanization is carried out in steps a, b, c, and d, control the rate at which the boat enters the fully automatic boat pushing furnace production line to be 1-2 h / boat.

7. The method for continuous high-temperature solid-phase synthesis of cobalt disulfide powder according to claim 1, characterized in that: In step a, the total cobalt content in semi-finished product 1 is ≤58%; in step b, the total cobalt content in semi-finished product 2 is ≤52%; in step c, the total cobalt content in semi-finished product 3 is ≤50%.

8. The method for continuous high-temperature solid-phase synthesis of cobalt disulfide powder according to claim 1, characterized in that: A sulfur recovery device is installed. After each sulfurization process, excess sulfur powder is vaporized at high temperature for 3 hours and then collected in the sulfur recovery device along with pure nitrogen.

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