CN101850965A - Spherical graphite with median diameter of 11 to 16 mu m and preparation method thereof - Google Patents
Spherical graphite with median diameter of 11 to 16 mu m and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of spherical graphite with a median diameter of 11 to 16 mu m. A five-level powder refining machine set consisting of an air-flow vortex powder refining machine and a cyclone separator is sequentially connected with a fourteen-level nodulizing machine set consisting of an air-flow vortex nodulizing machine and a nodulizing classifier in series; the graphite material enters from the first powder refining machine set and then flows through the five powder refining machine sets and the fourteen nodulizing machine sets in turn and finally out of the last nodulizing machine set; and by refining and nodulizing the powder, the spherical graphite product is obtained. The tap density of the obtained spherical graphite is 1.07-1.10 g/ml, and the number of openings on the surface of the graphite powder is 9-80 per mu m. The sphericity of the product is high, the electrochemical performance is obviously improved, the battery capacity, the standby time and the service life are effectively increased, and no overheat happens; moreover, the preparation method can improve the yield by over 75 percent, lower the cost by 38 percent, save the power consumption by 42 percent and realize the dust recovery rate up to 100%.
Description
Technical field
The present invention relates to a kind of Graphite Powder 99, specifically a kind of meso-position radius is spherical graphite of 11-16 μ m and preparation method thereof.
Background technology
Graphite material has good electrical conductivity, good charging/discharging voltage platform, higher specific storage and cheap advantages such as price as lithium ion battery negative material, so be the research focus of negative material always, in the commercialization lithium ion battery, be extensive use of.Many studies show that, the shape of graphite granule, crystalline structure, surface tissue, foreign matter content etc. all have substantial connection with the chemical property and the embedding lithium performance of graphite material.And the source of graphite is different with the course of processing, and its above-mentioned physical and chemical performance is also different.The structure of electrode materials itself is an important factor of decision lithium ion battery high power charging-discharging ability, so in research and production process, wish to get the well behaved graphite cathode material of embedding lithium, just its many-sided physical and chemical index must be effectively controlled, the good comprehensive properties electrode materials could be obtained.The electrical property that the spheroidization of graphite granule is handled improving natural graphite powder has great significance, and the graphite granule sphericity is good more, and electrical property is just good more.And existing spherical graphite is because its preparation technology's restriction, produce that productive rate is low, energy consumption is big, cost is high, and it is not high to make the sphericity of spherical graphite, the performance of product is undesirable, can't satisfy the needs of technical development, cause the time that discharges and recharges, standby time and the work-ing life of battery undesirable.Also cause charging capacity little when using as the power vehicle battery, easily produce superheating phenomenon, security and practicality are low.Chinese patent application numbers 97193389.8 discloses a kind of Graphite Powder 99 of using of being suitable in the negative pole of lithium-ion secondary cell, have the layering form of the C plane layer being made of several in the lip-deep closed ends structure of Graphite Powder 99 (surperficial closed ends structure), the C plane layer is closed at its place, end around adjoining course.Between two adjacent layering closed ends structures, maintain in C plane layer open-ended one " space ", the density of clearance gap (corresponding to the density of layering closed ends structure) remarkably influenced has the loading capacity of the lithium-ion secondary cell of the negative pole that Graphite Powder 99 forms.But it requires Graphite Powder 99 to have very little specific surface area, and specific surface area is crossed the young pathbreaker and caused reducing of battery reversible capacity.
Tap density, the i.e. quality of the measured unit volume after jolt ramming of the powder in the container under prescribed condition.The tap density size of spherical graphite is the important factor that influences its performance.
Summary of the invention
Technical problem to be solved by this invention provides the preparation method of the spherical graphite of a kind of meso-position radius 11-16 μ m, and the spherical graphite product sphericity height, the chemical property that make are good.
The present invention solves the problems of the technologies described above the technical scheme that is adopted to be: the preparation method of the spherical graphite of meso-position radius 11-16 μ m, the Pyatyi powder refinement unit that employing is made up of air-flow vortex powder refinement machine and air-flow vortex separator, be connected in series in proper order with the ten level Four nodularization units of being made up of air-flow vortex balling machine and nodularization sorting equipment, the preparation method is as follows:
Step 1, with particle diameter is 50 orders--325 orders, the crystalline flake graphite raw material of carbon amount more than 60% sent into the thinning process that first step air-flow vortex powder refinement machine carries out powder, powder refinement dish rotating speed in the air-flow vortex powder refinement machine changes for per minute 2000-2950, internal classification machine wheel speed in the air-flow vortex powder refinement machine changes for per minute 50-400, after 1-5 minute, Graphite Powder 99 is sent into cyclonic separator, isolate the Graphite Powder 99 of particle diameter＞2.5 μ m, the Graphite Powder 99 of particle diameter＞2.5 μ m is sent into the thinning process that next stage air-flow vortex powder refinement machine continues to implement powder, and isolated graphite dust is sent into the pulse device for recovering powder;
Step 2, send into the thinning process that air-flow vortex powder refinement machine in the second stage continues to implement powder by the Graphite Powder 99 of the isolated particle diameter of step 1＞2.5 μ m, powder refinement dish rotating speed in the air-flow vortex powder refinement machine changes for per minute 2000-2950, internal classification machine wheel speed in the air-flow vortex powder refinement machine changes for per minute 300-600, the time of powder thinning process is 1-5 minute, Graphite Powder 99 through refinement is sent into cyclonic separator, isolate the Graphite Powder 99 of particle diameter＞2.5 μ m, the Graphite Powder 99 of particle diameter＞2.5 μ m is sent into the thinning process that next stage air-flow vortex powder refinement machine continues to implement powder, and isolated graphite dust is sent into the pulse device for recovering powder;
Step 3, implemented the thinning process of powder through the third stage and fourth stage air-flow vortex powder refinement machine successively and separated through cyclonic separator by the Graphite Powder 99 of the isolated particle diameter of step 2＞2.5 μ m, the refinement of its powder is identical with the described process of technical parameter and step 2 with isolating method;
Step 4, by the isolated particle diameter of step 3＞2.5 μ m Graphite Powder 99s, send into first step air-flow vortex balling machine and carry out nodularization, the rotating speed of air-flow vortex balling machine changes for per minute 3000-4800, wheel speed in the air-flow vortex balling machine changes for per minute 200-400, in air-flow vortex balling machine, utilize turbulent flow, the drive graphite particle of eddy current produces reunites, collision, friction, shearing action is carried out nodularization to Graphite Powder 99, after 1-3 minute, to send into the nodularization grading machine through the Graphite Powder 99 of nodularization, under the condition of wheel speed for per minute 3000-5200 commentaries on classics of nodularization grading machine, utilize turbulent flow, eddy current drives Graphite Powder 99 and implements to reunite, collision, friction and shunting, carry out secondary nodularization and classification, isolate the Graphite Powder 99 of particle diameter 2.5-42 μ m through the nodularization grading machine, the Graphite Powder 99 of particle diameter 2.5-42 μ m is sent into the next stage air-flow vortex balling machine and is continued nodularization, and isolated graphite dust is sent into the pulse device for recovering powder;
Step 5, by the isolated particle diameter of step 4 be the Graphite Powder 99 of 2.5-42 μ m successively through 13 grades of air-flow vortex balling machines in the second stage to the and nodularization grading machine, its nodularization is identical with the described process of technical parameter and step 4 with the fractionated method;
Step 6, send into the tenth level Four air-flow vortex balling machine by the Graphite Powder 99 of the isolated particle diameter 2.5-42 of step 5 μ m and continue nodularization, the rotating speed of air-flow vortex balling machine changes for per minute 3200-4800, wheel speed in the air-flow vortex balling machine changes for per minute 300-500, after 1-3 minute, Graphite Powder 99 is sent into the nodularization grading machine carry out secondary nodularization and classification, the wheel speed of nodularization grading machine changes for per minute 3500-5400, isolate the Graphite Powder 99 that particle diameter is 2.5-40 μ m through the nodularization grading machine, particle diameter is that the Graphite Powder 99 of 2.5-40 μ m flows into feed bin, be the spherical graphite product that the meso-position radius that makes is 11-16 μ m, isolated graphite dust flows into the pulse device for recovering powder.
Among the present invention, the spherical graphite that utilizes the preparation method of technique scheme to make, the employing natural flake graphite is made, has the closed end construction in surface, the graphite powder be shaped as sphere, the surface has opening, the meso-position radius of described spherical graphite powder is 11-16 μ m, its tap density is 1.07-1.10g/ml, and the open amount of Graphite Powder 99 surface is 9-80/μ m.
In the art, usually D50, D90 or D10 statement are adopted in the size distribution statement of graphite, wherein D represents the diameter of powder granule, and D50 represents the diameter (or claiming that 50% passes through particle diameter) of 50% of accumulative total, D10 represents the diameter of 10% of accumulative total, and D50 claims median size or meso-position radius again.The Graphite Powder 99 identical to meso-position radius, particle sphericity are good more, and the Graphite Powder 99 tap density is high more.
The invention has the beneficial effects as follows: by in the preparation process of technique scheme to the adjustment of equipment components rotating speed, utilize turbulent flow, the effect of eddy current drives the thinning process that Graphite Powder 99 is implemented powder earlier, after making its particle diameter be reduced to a certain degree, implement the nodularization process again, finally make spherical graphite with described tap density and surface tissue, its product sphericity height, has bigger tap density, chemistry and Heat stability is good, chemical property is significantly improved, not only can be used as lithium ion battery negative material, also can become the starting material of isotropic graphite high-end products such as nuclear graphite.Have good embedding lithium performance as graphite cathode material, can reversible to greatest extent removal lithium embedded ion, the reversible capacity first and the coulombic efficiency of graphite cathode obviously improve.Effectively improved cell container, standby time and work-ing life, and can not produce superheating phenomenon, security and practicality are good.This preparation method compares with traditional method and can improve productive rate more than 75%, reduces cost 38%, and current consumption saves 42%, the dust rate of recovery 100%.
Embodiment
The preparation method of the spherical graphite of meso-position radius 11-16 μ m, the Pyatyi powder refinement unit that employing is made up of air-flow vortex powder refinement machine and cyclonic separator, be connected in series in proper order with the ten level Four nodularization units of forming by air-flow vortex balling machine and nodularization sorting equipment, graphite raw material is entered by first powder refinement unit, flow through successively behind five powder refinement units and 14 the nodularization units, flowed out by last nodularization unit, graphite raw material makes the spherical graphite product through the refinement and the nodularization process of powder.The powder refinement unit that is provided with and the group number of nodularization unit also can be adjusted as required.The spherical graphite product that makes has the closed end construction in surface, the graphite powder be shaped as sphere, the surface has opening, its tap density is 1.07-1.10g/ml, the open amount of Graphite Powder 99 surface is 9-80/μ m.
The air-flow vortex powder refinement machine of powder refinement unit can be selected QWJ-60 type air-flow vortex pulverizing mill for use in technique scheme, and the air-flow vortex balling machine of nodularization unit can be selected QWJ-30 type air-flow vortex pulverizing mill for use.Selected air-flow vortex powder refinement machine and air-flow vortex balling machine, its inside has rotating disk (being powder refinement dish) and internal classification impeller, the body inwall is provided with the gear ring corresponding with rotating disk, graphite raw material is delivered to the rotating disk below from opening for feed, drive the internal classification impeller that the slit of passing between rotating disk and the gear ring arrives body upper by air-flow, qualified Graphite Powder 99 flows out from discharge port by impeller, thicker graphite granule is then thrown away by impeller and is fallen, and Graphite Powder 99 acts in the body constantly circulation with the refinement (promptly reducing particle diameter) that reaches powder and the purpose of nodularization (being spheroidization) by air-flow.It is that micro mist prepares the common equipment in the classification process that cyclonic separator is called loading head again.Nodularization grading machine inside is provided with classifying turbine, and the centrifugal force that utilizes wind-force and impeller to produce makes Graphite Powder 99 carry out the process of nodularization and shunting in body.Air-flow vortex powder refinement machine, cyclonic separator, pulse device for recovering powder and negative pressure vacuum fan (can use high pressure centrifugal ventilator) are by airduct order serial connection in powder refinement unit; Air-flow vortex balling machine, nodularization grading machine, cyclonic separator, pulse device for recovering powder and negative pressure vacuum fan are by airduct order serial connection in the nodularization unit.The conveying of negative pressure in equipment that Graphite Powder 99 relies on negative-pressure air fan to produce.The motor that uses in the equipment can use speed control by frequency variation, does not have added losses, good energy-conserving effect in rotating speed control accuracy height, the speed regulation process.
Embodiment 1
The preparation method of the spherical graphite of meso-position radius 16 μ m, its preparation process is:
Step 1, with particle diameter is 50 orders--325 orders, the natural flake graphite raw material of carbon amount more than 60% sent into the thinning process that first step air-flow vortex powder refinement machine carries out powder, to reduce particle diameter, powder refinement dish rotating speed in the air-flow vortex powder refinement machine is that per minute 2300 changes, internal classification machine wheel speed in the air-flow vortex powder refinement machine is that per minute 200 changes, after 60 seconds, Graphite Powder 99 is sent into cyclonic separator, isolate the Graphite Powder 99 of particle diameter＞5 μ m, the Graphite Powder 99 of particle diameter＞5 μ m is sent into the thinning process that next stage air-flow vortex powder refinement machine continues to implement powder, and isolated graphite dust is sent into the pulse device for recovering powder;
Step 2, send into the thinning process that air-flow vortex powder refinement machine in the second stage continues to implement powder by the Graphite Powder 99 of the isolated particle diameter of step 1＞5 μ m, powder refinement dish rotating speed in the air-flow vortex powder refinement machine is that per minute 2300 changes, internal classification machine wheel speed in the air-flow vortex powder refinement machine is that per minute 300 changes, the time of powder thinning process is 50 seconds, Graphite Powder 99 through refinement is sent into cyclonic separator, isolate the Graphite Powder 99 of particle diameter＞5 μ m, the Graphite Powder 99 of particle diameter＞5 μ m is sent into the thinning process that next stage air-flow vortex powder refinement machine continues to implement powder, and isolated graphite dust is sent into the pulse device for recovering powder;
Step 3, implemented the thinning process of powder through the third stage and fourth stage air-flow vortex powder refinement machine successively and separated through cyclonic separator by the Graphite Powder 99 of the isolated particle diameter of step 2＞5 μ m, the refinement of its powder is identical with the described process of technical parameter and step 2 with isolating method;
Step 4, by the isolated particle diameter of step 3＞5 μ m Graphite Powder 99s, send into first step air-flow vortex balling machine and carry out nodularization, the rotating speed of air-flow vortex balling machine is that per minute 3000 changes, wheel speed in the air-flow vortex balling machine is that per minute 200 changes, in air-flow vortex balling machine, utilize turbulent flow, the drive graphite particle of eddy current produces reunites, collision, friction, shearing action is carried out nodularization to Graphite Powder 99, after 40 seconds, to send into the nodularization grading machine through the Graphite Powder 99 of nodularization, at the wheel speed of nodularization grading machine is to utilize turbulent flow under per minute 5200 condition of changeing, eddy current drives Graphite Powder 99 and implements to reunite, collision, friction and shunting, carry out secondary nodularization and classification, isolate the Graphite Powder 99 of particle diameter 5-42 μ m through the nodularization grading machine, the Graphite Powder 99 of particle diameter 5-42 μ m is sent into the next stage air-flow vortex balling machine and is continued nodularization, and isolated graphite dust is sent into the pulse device for recovering powder;
Step 5, by the isolated particle diameter of step 4 be the Graphite Powder 99 of 5-42 μ m successively through 13 grades of air-flow vortex balling machines in the second stage to the and nodularization grading machine, its nodularization is identical with the described process of technical parameter and step 4 with the fractionated method;
Step 6, send into the tenth level Four air-flow vortex balling machine by the Graphite Powder 99 of the isolated particle diameter 5-42 of step 5 μ m and continue nodularization, the rotating speed of air-flow vortex balling machine is that per minute 3200 changes, wheel speed in the air-flow vortex balling machine is that per minute 300 changes, after 35 seconds, Graphite Powder 99 is sent into the nodularization grading machine carry out secondary nodularization and classification, the wheel speed of nodularization grading machine is that per minute 3500 changes, isolate the Graphite Powder 99 that particle diameter is 5-40 μ m through the nodularization grading machine, particle diameter is that the Graphite Powder 99 of 5-40 μ m flows into feed bin, being the meso-position radius that makes is 16 μ m, tap density is 1.07g/ml, the open amount on surface is the spherical graphite product of 55-80/μ m, and isolated graphite dust flows into the pulse device for recovering powder.The spherical graphite that makes has the closed end construction in surface, the graphite powder be shaped as sphere, the surface has opening, its tap density is 1.07g/ml, the open amount on surface is 55-80/μ m.
Embodiment 2
A kind of spherical graphite, meso-position radius are 14 μ m, and tap density is 1.08g/ml, and the open amount of Graphite Powder 99 surface is 30～65/μ m, and its preparation method is:
Step 1, with particle diameter is 50 orders--325 orders, the natural flake graphite raw material of carbon amount more than 60% sent into the thinning process that first step air-flow vortex powder refinement machine is implemented powder, to reduce particle diameter, powder refinement dish rotating speed in the air-flow vortex powder refinement machine is that per minute 2500 changes, internal classification machine wheel speed in the air-flow vortex powder refinement machine is that per minute 150 changes, after 50 seconds, Graphite Powder 99 is sent into cyclonic separator, isolate the Graphite Powder 99 of particle diameter＞4 μ m, the Graphite Powder 99 of particle diameter＞4 μ m is sent into the thinning process that next stage air-flow vortex powder refinement machine continues to implement powder, and isolated graphite dust is sent into the pulse device for recovering powder;
Step 2, send into the thinning process that air-flow vortex powder refinement machine in the second stage continues to implement powder by the Graphite Powder 99 of the isolated particle diameter of step 1＞4 μ m, powder refinement dish rotating speed in the air-flow vortex powder refinement machine is that per minute 2500 changes, internal classification machine wheel speed in the air-flow vortex powder refinement machine is that per minute 380 changes, the time of powder thinning process is 60 seconds, Graphite Powder 99 through refinement is sent into cyclonic separator, isolate the Graphite Powder 99 of particle diameter＞4 μ m, the Graphite Powder 99 of particle diameter＞4 μ m is sent into the thinning process that next stage air-flow vortex powder refinement machine continues to implement powder, and isolated graphite dust is sent into the pulse device for recovering powder;
Step 3, implemented the thinning process of powder through the third stage and fourth stage air-flow vortex powder refinement machine successively and separated through cyclonic separator by the Graphite Powder 99 of the isolated particle diameter of step 2＞4 μ m, its powder refinement is identical with the described process of technical parameter and step 2 with isolating method;
Step 4, by the isolated particle diameter of step 3＞4 μ m Graphite Powder 99s, send into first step air-flow vortex balling machine and carry out nodularization, the rotating speed of air-flow vortex balling machine is that per minute 3400 changes, wheel speed in the air-flow vortex balling machine is that per minute 280 changes, in air-flow vortex balling machine, utilize turbulent flow, the drive graphite particle of eddy current produces reunites, collision, friction, shearing action is carried out nodularization to Graphite Powder 99, after 30 seconds, to send into the nodularization grading machine through the Graphite Powder 99 of nodularization, at the wheel speed of nodularization grading machine is to utilize turbulent flow under per minute 3800 condition of changeing, eddy current drives Graphite Powder 99 and implements to reunite, collision, friction and shunting, carry out secondary nodularization and classification, isolate the Graphite Powder 99 of particle diameter 4-40 μ m through the nodularization grading machine, the Graphite Powder 99 of particle diameter 4-40 μ m is sent into the next stage air-flow vortex balling machine and is continued nodularization, and isolated graphite dust is sent into the pulse device for recovering powder;
Step 5, by the isolated particle diameter of step 4 be the Graphite Powder 99 of 4-40 μ m successively through 13 grades of air-flow vortex balling machines in the second stage to the and nodularization grading machine, its nodularization is identical with the described process of technical parameter and step 4 with the fractionated method;
Step 6, send into the tenth level Four air-flow vortex balling machine by the Graphite Powder 99 of the isolated particle diameter 4-40 of step 5 μ m and continue nodularization, the rotating speed of air-flow vortex balling machine is that per minute 3500 changes, wheel speed in the air-flow vortex balling machine is that per minute 360 changes, after 45 seconds, Graphite Powder 99 is sent into the nodularization grading machine carry out secondary nodularization and classification, the wheel speed of nodularization grading machine is that per minute 4300 changes, isolate the Graphite Powder 99 that particle diameter is 4-38 μ m through the nodularization grading machine, particle diameter is that the Graphite Powder 99 of 4-38 μ m flows into feed bin, be the spherical graphite product that the meso-position radius that makes is 14 μ m, isolated graphite dust flows into the pulse device for recovering powder.The spherical graphite that makes has the closed end construction in surface, the graphite powder be shaped as sphere, the surface has opening, its tap density is 1.08g/ml, the open amount on surface is 30-65/μ m.
Embodiment 3
A kind of spherical graphite, meso-position radius are 12 μ m, and its tap density is 1.09g/ml, and the open amount of Graphite Powder 99 surface is 15-55/μ m, and its preparation method is:
Step 1, with particle diameter is 50 orders--325 orders, the natural flake graphite raw material of carbon amount more than 60% sent into the thinning process that first step air-flow vortex powder refinement machine is implemented powder, to reduce particle diameter, powder refinement dish rotating speed in the air-flow vortex powder refinement machine is that per minute 2700 changes, internal classification machine wheel speed in the air-flow vortex powder refinement machine is that per minute 300 changes, after 40 seconds, Graphite Powder 99 is sent into cyclonic separator, isolate the Graphite Powder 99 of particle diameter＞3 μ m, the Graphite Powder 99 of particle diameter＞3 μ m is sent into the thinning process that next stage air-flow vortex powder refinement machine continues to implement powder, and isolated graphite dust is sent into the pulse device for recovering powder;
Step 2, send into the thinning process that air-flow vortex powder refinement machine in the second stage continues to implement powder by the Graphite Powder 99 of the isolated particle diameter of step 1＞3 μ m, powder refinement dish rotating speed in the air-flow vortex powder refinement machine is that per minute 2950 changes, internal classification machine wheel speed in the air-flow vortex powder refinement machine is that per minute 450 changes, the time of powder thinning process is 50 seconds, Graphite Powder 99 through refinement is sent into cyclonic separator, isolate the Graphite Powder 99 of particle diameter＞3 μ m, the Graphite Powder 99 of particle diameter＞3 μ m is sent into the thinning process that next stage air-flow vortex powder refinement machine continues to implement powder, and isolated graphite dust is sent into the pulse device for recovering powder;
Step 3, implemented the thinning process of powder through the third stage and fourth stage air-flow vortex powder refinement machine successively and separated through cyclonic separator by the Graphite Powder 99 of the isolated particle diameter of step 2＞3 μ m, its powder refinement is identical with the described process of technical parameter and step 2 with isolating method;
Step 4, by the isolated particle diameter of step 3＞3 μ m Graphite Powder 99s, send into first step air-flow vortex balling machine and carry out nodularization, the rotating speed of air-flow vortex balling machine is that per minute 4000 changes, wheel speed in the air-flow vortex balling machine is that per minute 400 changes, in air-flow vortex balling machine, utilize turbulent flow, the drive graphite particle of eddy current produces reunites, collision, friction, shearing action is carried out nodularization to Graphite Powder 99, after 50 seconds, to send into the nodularization grading machine through the Graphite Powder 99 of nodularization, at the wheel speed of nodularization grading machine is to utilize turbulent flow under per minute 4500 condition of changeing, eddy current drives Graphite Powder 99 and implements to reunite, collision, friction and shunting, carry out secondary nodularization and classification, isolate the Graphite Powder 99 of particle diameter 3-38 μ m through the nodularization grading machine, the Graphite Powder 99 of particle diameter 3-38 μ m is sent into the next stage air-flow vortex balling machine and is continued nodularization, and isolated graphite dust is sent into the pulse device for recovering powder;
Step 5, by the isolated particle diameter of step 4 be the Graphite Powder 99 of 3-38 μ m successively through 13 grades of air-flow vortex balling machines in the second stage to the and nodularization grading machine, its nodularization is identical with the described process of technical parameter and step 4 with the fractionated method;
Step 6, send into the tenth level Four air-flow vortex balling machine by the Graphite Powder 99 of the isolated particle diameter 3-38 of step 5 μ m and continue nodularization, the rotating speed of air-flow vortex balling machine is that per minute 4200 changes, wheel speed in the air-flow vortex balling machine is that per minute 420 changes, after 55 seconds, Graphite Powder 99 is sent into the nodularization grading machine carry out secondary nodularization and classification, the wheel speed of nodularization grading machine is that per minute 4500 changes, isolate the Graphite Powder 99 that particle diameter is 3-35 μ m through the nodularization grading machine, particle diameter is that the Graphite Powder 99 of 3-35 μ m flows into feed bin, be the spherical graphite product that the meso-position radius that makes is 12 μ m, isolated graphite dust flows into the pulse device for recovering powder.The spherical graphite that makes has the closed end construction in surface, the graphite powder be shaped as sphere, the surface has opening, its tap density is 1.09g/ml, the open amount on surface is 15-55/μ m.
Embodiment 4
A kind of spherical graphite, meso-position radius are 11 μ m, and its tap density is 1.10g/ml, and the open amount of Graphite Powder 99 surface is 9～30/μ m, and its preparation method is:
Step 1, with particle diameter is 50 orders--325 orders, the natural flake graphite raw material of carbon amount more than 60% sent into the thinning process that first step air-flow vortex powder refinement machine is implemented powder, to reduce particle diameter, powder refinement dish rotating speed in the air-flow vortex powder refinement machine is that per minute 2950 changes, internal classification machine wheel speed in the air-flow vortex powder refinement machine is that per minute 300 changes, after 35 seconds, Graphite Powder 99 is sent into cyclonic separator, isolate the Graphite Powder 99 of particle diameter＞2.5 μ m, the Graphite Powder 99 of particle diameter＞2.5 μ m is sent into the thinning process that next stage air-flow vortex powder refinement machine continues to implement powder, and isolated graphite dust is sent into the pulse device for recovering powder;
Step 2, send into the thinning process that air-flow vortex powder refinement machine in the second stage continues to implement powder by the Graphite Powder 99 of the isolated particle diameter of step 1＞2.5 μ m, powder refinement dish rotating speed in the air-flow vortex powder refinement machine is that per minute 2700 changes, internal classification machine wheel speed in the air-flow vortex powder refinement machine is that per minute 600 changes, the time of powder thinning process is 30 seconds, Graphite Powder 99 through refinement is sent into cyclonic separator, isolate the Graphite Powder 99 of particle diameter＞2.5 μ m, the Graphite Powder 99 of particle diameter＞2.5 μ m is sent into the thinning process that next stage air-flow vortex powder refinement machine continues to implement powder, and isolated graphite dust is sent into the pulse device for recovering powder;
Step 3, implemented the thinning process of powder through the third stage and fourth stage air-flow vortex powder refinement machine successively and separated through cyclonic separator by the Graphite Powder 99 of the isolated particle diameter of step 2＞2.5 μ m, its powder refinement is identical with the described process of technical parameter and step 2 with isolating method;
Step 4, by the isolated particle diameter of step 3＞2.5 μ m Graphite Powder 99s, send into first step air-flow vortex balling machine and carry out nodularization, the rotating speed of air-flow vortex balling machine is that per minute 4800 changes, wheel speed in the air-flow vortex balling machine is that per minute 320 changes, in air-flow vortex balling machine, utilize turbulent flow, the drive graphite particle of eddy current produces reunites, collision, friction, shearing action is carried out nodularization to Graphite Powder 99, after 60 seconds, to send into the nodularization grading machine through the Graphite Powder 99 of nodularization, at the wheel speed of nodularization grading machine is to utilize turbulent flow under per minute 5200 condition of changeing, eddy current drives Graphite Powder 99 and implements to reunite, collision, friction and shunting, carry out secondary nodularization and classification, isolate the Graphite Powder 99 of particle diameter 2.5-36 μ m through the nodularization grading machine, the Graphite Powder 99 of particle diameter 2.5-36 μ m is sent into the next stage air-flow vortex balling machine and is continued nodularization, and isolated graphite dust is sent into the pulse device for recovering powder;
Step 5, by the isolated particle diameter of step 4 be the Graphite Powder 99 of 2.5-36 μ m successively through 13 grades of air-flow vortex balling machines in the second stage to the and nodularization grading machine, its nodularization is identical with the described process of technical parameter and step 4 with the fractionated method;
Step 6, send into the tenth level Four air-flow vortex balling machine by the Graphite Powder 99 of the isolated particle diameter 2.5-36 of step 5 μ m and continue nodularization, the rotating speed of air-flow vortex balling machine is that per minute 4800 changes, wheel speed in the air-flow vortex balling machine is that per minute 500 changes, after 65 seconds, Graphite Powder 99 is sent into the nodularization grading machine carry out secondary nodularization and classification, the wheel speed of nodularization grading machine is that per minute 5400 changes, isolate the Graphite Powder 99 that particle diameter is 2.5-32 μ m through the nodularization grading machine, particle diameter is that the Graphite Powder 99 of 2.5-32 μ m flows into feed bin, be the spherical graphite product that the meso-position radius that makes is 11 μ m, isolated graphite dust flows into the pulse device for recovering powder.The spherical graphite that makes has the closed end construction in surface, the graphite powder be shaped as sphere, the surface has opening, its tap density is 1.10g/ml, the open amount on surface is 9-30/μ m.
Claims (2)
1. the preparation method of the spherical graphite of meso-position radius 11-16 μ m, the Pyatyi powder refinement unit that employing is made up of air-flow vortex powder refinement machine and cyclonic separator, be connected in series in proper order with the ten level Four nodularization units of being made up of air-flow vortex balling machine and nodularization sorting equipment, it is characterized in that: the preparation method is as follows:
Step 1, with particle diameter is 50 orders--325 orders, the crystalline flake graphite raw material of carbon amount more than 60% sent into the thinning process that first step air-flow vortex powder refinement machine carries out powder, powder refinement dish rotating speed in the air-flow vortex powder refinement machine changes for per minute 2300-2950, internal classification machine wheel speed in the air-flow vortex powder refinement machine changes for per minute 150-400,35-65 is after second, Graphite Powder 99 is sent into cyclonic separator, isolate the Graphite Powder 99 of particle diameter＞2.5 μ m, the Graphite Powder 99 of particle diameter＞2.5 μ m is sent into the thinning process that next stage air-flow vortex powder refinement machine continues to implement powder, and isolated graphite dust is sent into the pulse device for recovering powder;
Step 2, send into the thinning process that air-flow vortex powder refinement machine in the second stage continues to implement powder by the Graphite Powder 99 of the isolated particle diameter of step 1＞2.5 μ m, powder refinement dish rotating speed in the air-flow vortex powder refinement machine changes for per minute 2300-2950, internal classification machine wheel speed in the air-flow vortex powder refinement machine changes for per minute 300-500, the time of powder thinning process is 30-60 second, Graphite Powder 99 through refinement is sent into cyclonic separator, isolate the Graphite Powder 99 of particle diameter＞2.5 μ m, the Graphite Powder 99 of particle diameter＞2.5 μ m is sent into the thinning process that next stage air-flow vortex powder refinement machine continues to implement powder, and isolated graphite dust is sent into the pulse device for recovering powder;
Step 3, implemented the thinning process of powder through the third stage and fourth stage air-flow vortex powder refinement machine successively and separated through cyclonic separator by the Graphite Powder 99 of the isolated particle diameter of step 2＞2.5 μ m, the refinement of its powder is identical with the described process of technical parameter and step 2 with isolating method;
Step 4, by the isolated particle diameter of step 3＞2.5 μ m Graphite Powder 99s, send into first step air-flow vortex balling machine and carry out nodularization, the rotating speed of air-flow vortex balling machine changes for per minute 3000-4800, wheel speed in the air-flow vortex balling machine changes for per minute 200-400, in air-flow vortex balling machine, utilize turbulent flow, the drive graphite particle of eddy current produces reunites, collision, friction, shearing action is carried out nodularization to Graphite Powder 99,30-60 is after second, to send into the nodularization grading machine through the Graphite Powder 99 of nodularization, under the condition of wheel speed for per minute 3000-5200 commentaries on classics of nodularization grading machine, utilize turbulent flow, eddy current drives Graphite Powder 99 and implements to reunite, collision, friction and shunting, carry out secondary nodularization and classification, isolate the Graphite Powder 99 of particle diameter 2.5-42 μ m through the nodularization grading machine, the Graphite Powder 99 of particle diameter 2.5-42 μ m is sent into the next stage air-flow vortex balling machine and is continued nodularization, and isolated graphite dust is sent into the pulse device for recovering powder;
Step 5, by the isolated particle diameter of step 4 be the Graphite Powder 99 of 2.5-42 μ m successively through 13 grades of air-flow vortex balling machines in the second stage to the and nodularization grading machine, its nodularization is identical with the described process of technical parameter and step 4 with the fractionated method;
Step 6, send into the tenth level Four air-flow vortex balling machine by the Graphite Powder 99 of the isolated particle diameter 2.5-42 of step 5 μ m and continue nodularization, the rotating speed of air-flow vortex balling machine changes for per minute 3200-4800, wheel speed in the air-flow vortex balling machine changes for per minute 300-500,35-65 is after second, Graphite Powder 99 is sent into the nodularization grading machine carry out secondary nodularization and classification, the wheel speed of nodularization grading machine changes for per minute 3500-5400, isolate the Graphite Powder 99 that particle diameter is 2.5-40 μ m through the nodularization grading machine, particle diameter is that the Graphite Powder 99 of 2.5-40 μ m flows into feed bin, be the spherical graphite product that the meso-position radius that makes is 11-16 μ m, isolated graphite dust flows into the pulse device for recovering powder.
2. the spherical graphite that preparation method according to claim 1 makes, the employing natural flake graphite is made, has the closed end construction in surface, the graphite powder be shaped as sphere, the surface has opening, it is characterized in that: the meso-position radius of described spherical graphite powder is 11-16 μ m, and its tap density is 1.07-1.10g/ml, and the open amount of Graphite Powder 99 surface is 9-80/μ m.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102951633A (en) * | 2012-11-21 | 2013-03-06 | 芜湖浙鑫新能源有限公司 | Graphite spheroidization method and production system thereby |
| CN103801439A (en) * | 2014-02-17 | 2014-05-21 | 湖南省宁乡县长宁炭素制品有限公司 | High-speed crushing machine, and machining device and preparation method of ultra-micro graphite powder |
| RU2706623C1 (en) * | 2019-01-10 | 2019-11-19 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Ивановский государственный химико-технологический университет" | Method of producing particles of spherical graphite and device for its implementation |
| CN111747405A (en) * | 2020-07-09 | 2020-10-09 | 黑龙江省宝泉岭农垦溢祥新能源材料有限公司 | Production process of spherical graphite raw material |
| CN114178032A (en) * | 2021-12-09 | 2022-03-15 | 萝北奥星新材料有限公司 | Production method of spheroidized graphite with low specific surface area |
| CN115254370A (en) * | 2022-08-31 | 2022-11-01 | 浙江碳一新能源有限责任公司 | Spherical graphite and processing system and processing technology thereof |
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- 2009-11-27 CN CN200910172766A patent/CN101850965A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102951633A (en) * | 2012-11-21 | 2013-03-06 | 芜湖浙鑫新能源有限公司 | Graphite spheroidization method and production system thereby |
| CN103801439A (en) * | 2014-02-17 | 2014-05-21 | 湖南省宁乡县长宁炭素制品有限公司 | High-speed crushing machine, and machining device and preparation method of ultra-micro graphite powder |
| CN103801439B (en) * | 2014-02-17 | 2016-04-13 | 湖南省宁乡县长宁炭素制品有限公司 | The process equipment of high speed disintegrator and ultra micro graphite powder |
| RU2706623C1 (en) * | 2019-01-10 | 2019-11-19 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Ивановский государственный химико-технологический университет" | Method of producing particles of spherical graphite and device for its implementation |
| CN111747405A (en) * | 2020-07-09 | 2020-10-09 | 黑龙江省宝泉岭农垦溢祥新能源材料有限公司 | Production process of spherical graphite raw material |
| CN114178032A (en) * | 2021-12-09 | 2022-03-15 | 萝北奥星新材料有限公司 | Production method of spheroidized graphite with low specific surface area |
| CN115254370A (en) * | 2022-08-31 | 2022-11-01 | 浙江碳一新能源有限责任公司 | Spherical graphite and processing system and processing technology thereof |
| CN115254370B (en) * | 2022-08-31 | 2024-03-01 | 碳一新能源集团有限责任公司 | Spherical graphite and processing system and processing technology thereof |
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