CN104627981A - Carbon product impregnation technology - Google Patents
Carbon product impregnation technology Download PDFInfo
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- CN104627981A CN104627981A CN201510077747.1A CN201510077747A CN104627981A CN 104627981 A CN104627981 A CN 104627981A CN 201510077747 A CN201510077747 A CN 201510077747A CN 104627981 A CN104627981 A CN 104627981A
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- graphite powder
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Abstract
The invention relates to the field of graphite material production and in particular relates to a carbon product impregnation technology which can completely impregnate graphite powder into a carbon product. The carbon product impregnation technology comprises the following steps: firstly selecting low-quinoline insoluble impregnant asphalt, secondly putting the low-quinoline insoluble impregnant asphalt into an impregnation tank, thirdly adding high-quality and natural graphite powder or artificial graphite powder into the impregnant asphalt, preheating a carbon product, then carrying out impregnation, pressurization and impregnation, and then carrying out water cooling. When the carbon product impregnation technology is adopted for impregnating the carbon product, number impregnation times can be reduced, a production period can be shortened, production cost can be reduced, temperature heat transmission uniformity during roasting is improved due to impregnation of the high-purity graphite powder, and the graphite powder has good heat conductivity, so that yield of the product is also effectively increased in the roasting process.
Description
Technical field
The present invention relates to graphite material production field, be specifically related to a kind of impregnation technology that Graphite Powder 99 can be immersed into completely the carbon goods in carbon goods.
Background technology
Complex process in carbon graphite article manufacturing process and operation is more, the discharge of particularly a large amount of in roasting process fugitive constituents causes a large amount of fugitive constituents of cakingagent pitch to discharge, make the performance change of carbon goods, volume density, strength degradation, void content increases, thus affects every physical index of graphite product.
Now in process of production, for making up fugitive constituent loss, causing product defect, being all make up product defect with repeatedly dipping process and calcining process, causing the raising of production cost.Because China's Carbon Materials industry adopts mid-temperature pitch cakingagent softening point temperature low (75-95 DEG C) β resin content less always, cakingagent performance is not ideal enough, and after carbonization, coking value is general lower, between 45-50%.The high-end carbon material production of production high strength and Gao Timi is just not suitable for.For the quality improving carbon material must select good cohesiveness and higher coking value fat coal pitch to be used as soaker.The present feature that modified pitch cohesiveness is good, coking value is high, but the poor fluidity of modified pitch, suitable end viscosity temperature range narrows, bring a lot of problems in actual applications, one is that pitch dissolves and carries, thickener kneading and mold temperature all will improve greatly in addition, and the scope of mobility and thickener plasticity more embarrasses control, directly affect the ratio of briquetting of carbon goods and the yield rate in later stage.
Summary of the invention
The object of the invention is to overcome deficiency of the prior art and the impregnation technology that a kind of carbon goods are provided, this process increases the carburetting rate of carbon goods, volume density, intensity, decrease void content.
The object of the present invention is achieved like this:
An impregnation technology for carbon goods, technique is as follows:
First select the dipping agent bitumen of low quinoline insolubles, then be contained in impregnating autoclave, then high-quality natural graphite powder or graphous graphite powder, join in dipping agent bitumen, add according to the part by weight of mixing rear 30%, by stirring, high-quality natural graphite powder or graphous graphite powder are mixed in dipping agent bitumen uniformly again, then needing the carbon goods of dipping to carry out preheating under 220-250 DEG C of condition, preheated carbon goods put into impregnating autoclave in 15-20 minute, 0.096Mpa is evacuated to impregnating autoclave, pressurize 3-4.5 hour, then in impregnating autoclave, inject the dipping agent bitumen of 140-155 DEG C that modulates, then pressurize, impregnation pressure is 1.45-1.6Mpa, dipping time is 2-3 hour, water cooling is carried out to the carbon goods after dipping, water-cooled temperature is 30-45 DEG C, cooling time is 2 hours, make the abundant coking in the process of roasting of the carbon goods after dipping.
Based on the above, described natural graphite powder or the purity of graphous graphite powder are 99.9%, and granularity is 0.5-2 μm, select 99.9% Graphite Powder 99 to be that impurity only has 0.1% weight ratio, thus adds the content of carbon because the carbon content of carbon goods itself is higher.After another Graphite Powder 99 immerses, first coking value (carbon content) that can increase carbon goods, second physical strength that can increase carbon goods, 3rd in roasting process carbon goods be heated evenly and can improve carbon goods yield rate, the 4th carbon goods finally will carry out 2800 DEG C of high temperature graphitizations (synthetic graphite).Talk material and belong to porous material, the total porosity of carbon goods is 25-32%, the total porosity 16-25% of graphite product, select granularity 0.5-2 μm, because measuring carbon goods air vent aperture 5-8 μm at powerful microscope, select granularity 0.5-2 μm to be in order to Graphite Powder 99 is immersed in carbon goods completely, because the granularity of Graphite Powder 99 is much smaller than the hole diameter of carbon goods, is convenient to Graphite Powder 99 like this and enters into inside the pore of carbon goods.
Based on the above, the quinoline insolubles weight content of the dipping agent bitumen of described low quinoline insolubles is at 5-10%, the quinoline insolubles content of dipping agent bitumen should be lower, the immersion rate of pitch is reduced because quinoline insolubles easily forms impervious filter cake at goods void entry, too high levels will reduce the bond performance of pitch on the other hand, is that coal-tar pitch mobility is deteriorated thus affects dipping effect.
Quinoline insolubles is lower, relation is had with the binding agent wettability of pitch, its wettability is better, just and combine between the inner powder of carbon goods better, moreover it is inseparable with the perviousness of dipping agent bitumen, soaker can be made to immerse in the internal capillary of powder, thus make together with the good goods of dipping " to inlay " with goods powder in the program roasting process soaker coking of lower road, the intensity of more favourable raising carbon goods.
Calculating by following: the high-purity graphite powder of 30% is stayed in goods, 70% amount of dipping agent bitumen then has the coking value of 49%.10KG is the pitch amount immersing every block goods, and 30% adds ratio for Graphite Powder 99, and 70% is pitch adds ratio, the dipping agent bitumen be mixed into, and 49% is the coking value of pitch.Calculate by immersion 10kg pitch, (30% × 10kg+10 × 70% × 49%)/10 × 49%=1.31%, the carbon goods carburetting rate after baking of the soaker after improvement improves the carbon increasing amount of 31%.
The present invention has following advantage:
Invention increases the capability and performance of carbon goods, volume density, intensity improve greatly, and void content is less.Dipping number of times can be reduced with this method impregnated carbon goods, shorten the production cycle, reduce production cost.When the immersion of another high purity graphite powder improves roasting, the homogeneity (Graphite Powder 99 has good thermal conductivity) of temperature heat transfer, also effectively can improve the yield rate of product at calcining process.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1:
An impregnation technology for carbon goods, technique is as follows:
First select common conventional dipping agent bitumen, then be contained in impregnating autoclave, then high-quality natural graphite powder or graphous graphite powder, join in dipping agent bitumen, add according to the part by weight of mixing rear 30%, by stirring, high-quality natural graphite powder or graphous graphite powder are mixed in dipping agent bitumen uniformly again, then needing the carbon goods of dipping to carry out preheating under 240 DEG C of conditions, preheated carbon goods put into impregnating autoclave in 15-20 minute, 0.096Mpa is evacuated to impregnating autoclave, pressurize 3-4.5 hour, then in impregnating autoclave, inject the dipping agent bitumen of 140-155 DEG C that modulates, then pressurize, impregnation pressure is 1.45-1.6Mpa, dipping time is 2-3 hour, water cooling is carried out to the carbon goods after dipping, water-cooled temperature is 30-45 DEG C, cooling time is 2 hours, make the abundant coking in the process of roasting of the carbon goods after dipping.
Embodiment 2:
An impregnation technology for carbon goods, technique is as follows:
First select the dipping agent bitumen of low quinoline insolubles, then be contained in impregnating autoclave, then high-quality natural graphite powder or graphous graphite powder, join in dipping agent bitumen, add according to the part by weight of mixing rear 30%, by stirring, high-quality natural graphite powder or graphous graphite powder are mixed in dipping agent bitumen uniformly again, then needing the carbon goods of dipping to carry out preheating under 240 DEG C of conditions, preheated carbon goods put into impregnating autoclave in 15-20 minute, 0.096Mpa is evacuated to impregnating autoclave, pressurize 3-4.5 hour, then in impregnating autoclave, inject the dipping agent bitumen of 155 DEG C that modulate, then pressurize, impregnation pressure is 1.45-1.6Mpa, dipping time is 2-3 hour, water cooling is carried out to the carbon goods after dipping, water-cooled temperature is 30-45 DEG C, cooling time is 2 hours, make the abundant coking in the process of roasting of the carbon goods after dipping.
The performance concrete analysis of indices is as follows:
1) fundamental property of low quinoline insolubles pitch and common conventional dipping agent bitumen is as table 1:
As can be seen from the table, the content of the quinoline insolubles of low quinoline insolubles pitch is starkly lower than the quinoline insolubles of common conventional dipping agent bitumen.
2) analysis of indices after low quinoline insolubles pitch and common conventional dipping agent bitumen dipping and contrast, as shown in Figure 2:
Can be found out by upper table: sample 2 namely adopts low quinoline insolubles pitch in embodiment, the close index of body of the carbon goods after dipping strengthens, and resistance to compression, folding strength obviously strengthen, and void content reduces, and yield rate is high.
Below in conjunction with the concrete analysis of the parameter index that preheating temperature, vacuum tightness, dipping temperature, impregnation pressure are concrete on the impact of carbon goods.
1) impregnation pressure impact that carbon goods are increased weight, when changing impregnation pressure, the maintenance that other technological factor is tried one's best is constant, and result is as shown in table 3:
As seen from Table 3, impregnation pressure increases to 1.6MPa weightening finish by 0.7MPa to be increased to some extent, and when more than 1.6MPa, weightening finish does not significantly change.As can be seen from the data of experiment, top condition when 1.45MPa-1.6MPa be can be used as bituminizing, only just can have a certain impact to weightening finish within the scope of certain pressure.
2) different preheating temperatures is on the impact of dipping weightening finish
Carbon goods are necessary preheating before dipping, otherwise do not reach the object of dipping, preheating temperature is mainly in order to shorten warm up time, warm up time is shorter, more favourable, but the temperature of preheating is too high, the oxidation of blank can be caused again, too low, warm up time is oversize, and preheating temperature adjustment of the present invention is 240 DEG C of the bests.As shown in Figure 1.
3) different vacuum tightness and vacuum tightness hold-time are on the impact of weightening finish
The condition of experimental selection is that vacuum tightness is with 7.6 × 10
4pa starts, every 0.4 × 10
4pa as a test point, until 9.6 × 10
4pa, as seen from Figure 2, along with the raising carbon goods weightening finish of vacuum tightness strengthens.
Change the impact of vacuum tightness hold-time on weightening finish, see the following form 4.
Hold-time longer as can be seen from the table can obtain higher weightening finish, and vacuum time continues 3-4.5 hour, but once more than 4.5 hours time, region substantially of increasing weight slowly selects suitable vacuum tightness necessary.
4) dipping temperature is on the impact of weightening finish
Dipping temperature to ensure that soaker has good flowing property under this condition, there is less viscosity, soaker is made to enter into carbon goods smoothly inner, can more be increased weight, but temperature is too high, also can be unfavorable for dipping, must be that soaker has good mobility and Li Qing can not carry out under the condition that great changes have taken place.As shown in chart 5,
As can be seen from Table 5, temperature is when 140-155 DEG C, and rate of body weight gain is the highest, also tends towards stability, and especially 155 DEG C time, rate of body weight gain reaches the highest.
Claims (3)
1. an impregnation technology for carbon goods, is characterized in that: technique is as follows:
First select the dipping agent bitumen of low quinoline insolubles, then be contained in impregnating autoclave, then high-quality natural graphite powder or graphous graphite powder, join in dipping agent bitumen, add according to the part by weight of mixing rear 30%, by stirring, high-quality natural graphite powder or graphous graphite powder are mixed in dipping agent bitumen uniformly again, then needing the carbon goods of dipping to carry out preheating under 220-250 DEG C of condition, preheated carbon goods put into impregnating autoclave in 15-20 minute, 0.096Mpa is evacuated to impregnating autoclave, pressurize 3-4.5 hour, then in impregnating autoclave, inject the dipping agent bitumen of 140-155 DEG C that modulates, then pressurize, impregnation pressure is 1.45-1.6Mpa, dipping time is 2-3 hour, water cooling is carried out to the carbon goods after dipping, water-cooled temperature is 30-45 DEG C, cooling time is 2 hours, make the abundant coking in the process of roasting of the carbon goods after dipping.
2. the impregnation technology of a kind of carbon goods according to claim 1, it is characterized in that: described natural graphite powder or the purity of graphous graphite powder are 99.9%, granularity is 0.5-2 μm.
3. the impregnation technology of a kind of carbon goods according to claim 1, is characterized in that: the quinoline insolubles weight content of the dipping agent bitumen of described low quinoline insolubles is at 5-10%.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106169584A (en) * | 2016-08-03 | 2016-11-30 | 深圳市贝特瑞新能源材料股份有限公司 | Graphite cathode material, preparation method and lithium ion battery |
CN107814383A (en) * | 2017-09-28 | 2018-03-20 | 广东东岛新能源股份有限公司 | A kind of lithium ion battery modification of microcrystalline graphite cathode material and its production and use |
CN114940628A (en) * | 2022-06-22 | 2022-08-26 | 湖南晶碳新材料有限公司 | A calcination article preprocessing device for flooding |
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CN101250724A (en) * | 2007-11-28 | 2008-08-27 | 温县东方炭素有限公司 | Method for producing one-dipping two-baking anode carbon block |
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CN101250724A (en) * | 2007-11-28 | 2008-08-27 | 温县东方炭素有限公司 | Method for producing one-dipping two-baking anode carbon block |
Non-Patent Citations (1)
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陈文燕等: "石油基浸渍沥青的制备综述", 《石油炼制与化工》 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106169584A (en) * | 2016-08-03 | 2016-11-30 | 深圳市贝特瑞新能源材料股份有限公司 | Graphite cathode material, preparation method and lithium ion battery |
CN106169584B (en) * | 2016-08-03 | 2019-06-07 | 深圳市贝特瑞新能源材料股份有限公司 | Modified graphite cathode material, preparation method and lithium ion battery |
CN107814383A (en) * | 2017-09-28 | 2018-03-20 | 广东东岛新能源股份有限公司 | A kind of lithium ion battery modification of microcrystalline graphite cathode material and its production and use |
CN114940628A (en) * | 2022-06-22 | 2022-08-26 | 湖南晶碳新材料有限公司 | A calcination article preprocessing device for flooding |
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