CN109665845A - 一种复合石墨电极的制备方法 - Google Patents
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Abstract
本发明公开一种复合石墨电极的制备方法,所述复合石墨电极的制备原料按质量计如下:25‑35份石油焦、18‑27份针状焦、9‑13份煤沥青、3‑8份的β‑SiC、1‑1.5份Fe2O3、0.6‑0.9份脂肪醇聚氧乙烯醚、0.4‑0.7份AL2O3、1‑3份铜粉、2‑4份碳酸钠Na2CO3。本发明利用粉碎机将上述原料粉碎为纳米级,纳米级粉料非常细小具有增加原料之间的接触面积,提高材料间的吸附性能,形成超薄的粘结薄膜和更具活性的焦粒,使骨料与焦粒间充分的结合,此结合力远远大于骨料直接跟粘结剂的结合力,从而形成更牢固的炭结构链,形成更强的结合体,另外,纳米级粉料能改善电极的性能,完善了电极的内部结构,确保了石墨电极的安全使用性能。
Description
技术领域
本发明涉及电极制备技术领域,具体是一种复合石墨电极的制备方法。
背景技术
石墨电极是指以石油焦、沥青焦为骨料,煤沥青为黏结剂,经过原料煅烧、破碎磨粉、配料、混捏、成型、焙烧、浸渍、石墨化和机械加工而制成的一种耐高温石墨质导电材料。其广泛应用于:电弧炼钢炉、用于矿热电炉、用于电阻炉和用于制备异型石墨产品。
目前石墨电极的制造工艺已经十分成熟和多样化,成品性能也比较高,但是各个厂家的制造工艺均属于保密状态或受专利保护,因此,需要进入石墨电极的制造领域就务必设计一种全新的、与现有技术有区别的制造工艺,但是目前,通过自行设计的制造工艺要么工艺复杂、成品率低,造成成本上涨,使得企业失去竞争力;要么产品质量差,使得企业竞争力较差。针对上述问题,本发明提出一种复合石墨电极的制备工艺,其工艺简单,且成本偏低,但是成品性能能够满足目前的需求。
发明内容
本发明的目的是在于提供一种复合石墨电极的制备方法,复合石墨电极的制备原料具体如下:石油焦、针状焦、煤沥青、三氧化二铁(Fe2O3)、脂肪醇聚氧乙烯醚(AEO)、氧化铝(AL2O3)、铜粉、碳酸钠(Na2CO3)。利用粉碎机将上述原料粉碎为纳米级,纳米级粉料非常细小具有增加原料之间的接触面积,提高材料间的吸附性能,形成超薄的粘结薄膜和更具活性的焦粒,使骨料与焦粒间充分的结合,此结合力远远大于骨料直接跟粘结剂的结合力,从而形成更牢固的炭结构链,形成更强的结合体,另外,纳米级粉料能改善电极的性能,完善了电极的内部结构,确保了石墨电极的安全使用性能,达到降低电极电阻率、提高抗氧化性能、抗折断性能、抗拉伸性能和延长电极使用周期寿命的目的。
本发明解决其技术问题所采用的技术方案是:
一种复合石墨电极,所述制备原料按质量计如下:
25-35份石油焦、18-27份针状焦、9-13份煤沥青、3-8份的β-SiC、1-1.5份Fe2O3、0.6-0.9份脂肪醇聚氧乙烯醚、0.4-0.7份AL2O3、1-3份铜粉、2-4份Na2CO3;
所述复合石墨电极的指标如下:5.5uΩ·m≦电阻率≦6.5uΩ.m,1.62g/cm3≦体积密度≦1.66g/cm3,10.5MPa≦抗折强度≦11MPa,12GPa≦弹性模量≦14GPa,1.5×10-6m/℃≦热膨胀系数≦2.4×10-6m/℃。
所述制备原料按质量计如下:25份石油焦、18份针状焦、9份煤沥青、3份的β-SiC、1份Fe2O3、0.6份脂肪醇聚氧乙烯醚、0.4份AL2O3、1份铜粉、2份Na2CO3。
所述制备原料按质量计如下:30份石油焦、23份针状焦、11份煤沥青、6份β-SiC、1.2份Fe2O3、0.8份脂肪醇聚氧乙烯醚、0.6份AL2O3、2份铜粉、3份Na2CO3。
所述制备原料按质量计如下:35份石油焦、27份针状焦、13份煤沥青、8份的β-SiC、1.5份Fe2O3、0.9份脂肪醇聚氧乙烯醚、0.7份AL2O3、3份铜粉、4份Na2CO3。
一种复合石墨电极的制备方法,所述具体步骤如下所示:
步骤一,原料粉碎,称取石油焦、针状焦、煤沥青、β-SiC、Fe2O3、AL2O3、铜粉和Na2CO3后,再利用粉碎机分别将其粉碎成纳米级粉末。
步骤二,原料筛分,利用气流筛分机对步骤一中粉碎的石油焦、针状焦、煤沥青、β-SiC、Fe2O3、AL2O3、铜粉和Na2CO3粉末分别进行筛分获得8-15nm的原料粉末。
步骤三,物料干混,称取石油焦、针状焦、和β-SiC纳米级粉末放入混捏锅内搅拌混合均匀,再依次加入Fe2O3、AL2O3、AL2O3和Na2CO3纳米级粉末以及脂肪醇聚氧乙烯醚搅拌进行干混。
步骤四,物料混捏,混捏完成后获得糊料。
步骤五,物料成型,将糊料放入成型机内,利用20MPa的压力将其压制成石墨电极半成品。
步骤六,石墨电极半成品焙烧,将石墨电极半成品放入环式焙烧炉内按照设计的升温曲线对其进行焙烧,并在最高温度1500℃保持25h后自然降温,冷却78h后获得石墨电极焙烧品。
步骤七,石墨电极焙烧品石墨化处理,将焙烧品放入石墨化炉内,按送电曲线对焙烧品进行石墨化处理,在此过程中,石墨化炉的温度加热至2800-3200℃,冷却维护时长控制在255-286h。
步骤八,质量指标检测,对石墨化品的电阻率、体积密度、抗折强度、弹性模量和热膨胀系数进行检测以判定石墨电极的质量。
步骤九,将石墨化品加工成规定规格的成品,而后按规定的匹配要求进行预组装、包装、入库。
所述步骤三中物料干混时混捏锅内搅拌器的搅拌速度为1200-1500r/min,干混时间为20-30min。
所述步骤四中物料混捏时混捏锅内温度升高至200-210℃,混捏时长控制在25-30min。
所述步骤五中,物料压制过程中成型机内温度为145-150℃,压制时长控制在3-3.5h。
所述步骤六中的升温包括八个阶段,八个阶段分别处于如下温区内:150-200℃、200-250℃、250-450℃、450-600℃、600-800℃、800-1200℃、1200-1500℃、1500。
所述步骤七送电曲线包括七个阶段,每个阶段的具体送电功率如下:2000KW、3000KW、4500KW、6500KW、8500KW、11500KW、13500KW。
本发明的有益效果是:
1、本发明将制备的原料粉碎为纳米级,纳米级粉料非常细小具有增加原料之间的接触面积,提高材料间的吸附性能,形成超薄的粘结薄膜和更具活性的焦粒,使骨料与焦粒间充分的结合,此结合力远远大于骨料直接跟粘结剂的结合力,从而形成更牢固的炭结构链,形成更强的结合体,另外,纳米级粉料能改善电极的性能,完善了电极的内部结构,确保了石墨电极的安全使用性能,达到降低电极电阻率、提高抗氧化性能、抗折断性能、抗拉伸性能和延长电极使用周期寿命的目的;
2、本发明添加了表面活性剂聚氧乙烯醚(AEO),AEO的极性基与焦粉表面的自出键相结合,缓解了焦粉表面的不饱和价力,AEO的亲油基与沥青分子相连,使得沥青表面分子的不均匀受力状况得到削弱,这种双重的“架桥”式作用的结果,降低了沥青的表面张力,进而降低了平衡接触角,提高了沥青对焦粉表面的湿涧性,颗粒间的粘结得到加强,从而提高制品的质量;
3、本发明添加了(AL2O3)以便促进石墨电极焙烧品的石墨化程度;
4、本发明中加入了β-SiC使得制备的石墨电极的耐磨、耐火、耐腐蚀、耐高温、导热性能和抗冲击性能都提高。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
一种复合石墨电极,其制备原料按质量计如下:
25-35份石油焦、18-27份针状焦、9-13份煤沥青、3-8份的β-SiC、1-1.5份三氧化二铁(Fe2O3)、0.6-0.9份脂肪醇聚氧乙烯醚(AEO)、0.4-0.7份氧化铝(AL2O3)、1-3份铜粉、2-4份碳酸钠(Na2CO3)。
一种复合石墨电极的制备方法,其具体步骤如下所示:
步骤一,原料粉碎,称取一定质量的石油焦、针状焦、煤沥青、β-SiC、Fe2O3、AL2O3、铜粉和Na2CO3后,再利用粉碎机分别将其粉碎成纳米级。
步骤二,原料筛分,利用气流筛分机对步骤一中粉碎的石油焦、针状焦、煤沥青、β-SiC、Fe2O3、AL2O3、铜粉和Na2CO3分别进行筛分获得8-15nm的原料粉末。
步骤三,物料干混,称取一定质量的石油焦、针状焦、和β-SiC放入混捏锅内搅拌混合均匀,再依次加入一定质量的Fe2O3、AL2O3、AEO、AL2O3和Na2CO3搅拌混合,搅拌速度1200-1500r/min,干混时间为20-30min。
步骤四,物料混捏,升高混捏锅内温度至200-210℃,对混捏锅内的物料混捏,混捏时长控制在25-30min,混捏完成后获得糊料。
步骤五,物料成型,将糊料放入成型机内,利用20MPa的压力将其压制成石墨电极半成品,在压制过程中,保持成型机内温度145-150℃,压制时长控制在3-3.5h。
步骤六,石墨电极半成品焙烧,将石墨电极半成品放入环式焙烧炉内按照设计的升温曲线如表1所示对其进行焙烧,并在最高温度1500℃保持25h后自然降温,冷却78h后获得石墨电极焙烧品。
表1焙烧升温曲线
阶段 | 温区(℃) | 升温速率(℃/h) | 持续时间(h) |
1 | 150-200 | 5.5 | 3.5 |
2 | 200-250 | 5.2 | 4.2 |
3 | 250-450 | 2.5 | 8.1 |
4 | 450-600 | 2.2 | 10.2 |
5 | 600-800 | 1.8 | 11.8 |
6 | 800-1200 | 1.5 | 13.5 |
7 | 1200-1500 | 1.1 | 16.8 |
8 | 1500 | -- | 25 |
步骤七,石墨电极焙烧品石墨化处理,将焙烧品放入石墨化炉内,按送电曲线如表2所示对焙烧品进行石墨化处理,在此过程中,石墨化炉的温度加热至2800-3200℃,冷却维护时长控制在255-286h。
表2送电曲线
阶段 | 送电时间(h) | 功率(KW) | 累计送电量(KWh) |
1 | 0-5 | 2000 | 2765 |
2 | 5-12 | 3000 | 3562 |
3 | 12-25 | 4500 | 11352 |
4 | 25-35 | 6500 | 14123 |
5 | 35-50 | 8500 | 35869 |
6 | 50-60 | 11500 | 67523 |
结束电量 | 60-70 | 13500 | 86921 |
步骤八,质量指标检测,对石墨化品的电阻率、体积密度、抗折强度、弹性模量和热膨胀系数进行检测以判定石墨电极的质量,对石墨化品的指标要求如下:
5.5uΩ.m≦电阻率≦6.5uΩ·m,1.62g/cm3≦体积密度≦1.66g/cm3,10.5MPa≦抗折强度≦11MPa,12GPa≦弹性模量≦14GPa,1.5×10-6m/℃≦热膨胀系数≦2.4×10-6m/℃。
步骤九,将石墨化品加工成规定规格的成品,而后按规定的匹配要求进行预组装、包装、入库。
实施示例
按上述制备方法来制备复合石墨电极。
实施例1:
称取25份石油焦、18份针状焦、9份煤沥青、3份β-SiC、1份Fe2O3、0.4份AL2O3、1份铜粉和2份Na2CO3后利用粉碎机分别将其粉碎成纳米级,再利用气流筛分机对粉碎的石油焦、针状焦、煤沥青、β-SiC、Fe2O3、AL2O3、铜粉和Na2CO3进行筛分获得8-15nm的原料粉末。
将上述石油焦、针状焦、和β-SiC粉末放入混捏锅内搅拌混合均匀,再依次加入一定质量的Fe2O3、AL2O3、AL2O3和Na2CO3粉末和0.6份AEO搅拌混合,搅拌速度为1200r/min,干混时间为20min。
将上述混合物料进行混捏,混捏锅内温度至200℃,混捏时长控制在25min,混捏完成后获得糊料,再将糊料放入成型机内,利用20MPa的压力将其压制成石墨电极半成品,在压制过程中,保持成型机内温度145℃,压制时长控制在3h。
对压制成型的石墨半成品按照焙烧曲线进行焙烧再自然冷却,冷却时长在78h。焙烧完后,取焙烧品进行石墨化处理,其中石墨化炉的温度加热至2800℃,冷却维护时长控制在255h。最后对石墨化品进行指标检测后再将其加工成规定规格的成品,而后按规定的匹配要求进行预组装、包装、入库。
实施例2:
称取30份石油焦、23份针状焦、11份煤沥青、6份β-SiC、1.2份Fe2O3、0.6份AL2O3、2份铜粉和3份Na2CO3后利用粉碎机分别将其粉碎成纳米级,再利用气流筛分机对粉碎的石油焦、针状焦、煤沥青、β-SiC、Fe2O3、AL2O3、铜粉和Na2CO3进行筛分获得8-15nm的原料粉末。
将上述石油焦、针状焦、和β-SiC粉末放入混捏锅内搅拌混合均匀,再依次加入一定质量的Fe2O3、AL2O3、AL2O3和Na2CO3粉末和0.8份AEO搅拌混合,搅拌速度为1350r/min,干混时间为25min。
将上述混合物料进行混捏,混捏锅内温度至205℃,混捏时长控制在28min,混捏完成后获得糊料,再将糊料放入成型机内,利用20MPa的压力将其压制成石墨电极半成品,在压制过程中,保持成型机内温度147℃,压制时长控制在3.3h。
对压制成型的石墨半成品按照焙烧曲线进行焙烧再自然冷却,冷却时长在78h。焙烧完后,取焙烧品进行石墨化处理,其中石墨化炉的温度加热至3000℃,冷却维护时长控制在265h。最后对石墨化品进行指标检测后再将其加工成规定规格的成品,而后按规定的匹配要求进行预组装、包装、入库。
实施例3:
称取35份石油焦、27份针状焦、13份煤沥青、8份β-SiC、1.5份Fe2O3、0.7份AL2O3、3份铜粉和4份Na2CO3后利用粉碎机分别将其粉碎成纳米级,再利用气流筛分机对粉碎的石油焦、针状焦、煤沥青、β-SiC、Fe2O3、AL2O3、铜粉和Na2CO3进行筛分获得8-15nm的原料粉末。
将上述石油焦、针状焦、和β-SiC粉末放入混捏锅内搅拌混合均匀,再依次加入一定质量的Fe2O3、AL2O3、AL2O3和Na2CO3粉末和0.9份AEO搅拌混合,搅拌速度为1500r/min,干混时间为30min。
将上述混合物料进行混捏,混捏锅内温度至210℃,混捏时长控制在30min,混捏完成后获得糊料,再将糊料放入成型机内,利用20MPa的压力将其压制成石墨电极半成品,在压制过程中,保持成型机内温度150℃,压制时长控制在3.5h。
对压制成型的石墨半成品按照焙烧曲线进行焙烧再自然冷却,冷却时长在78h。焙烧完后,取焙烧品进行石墨化处理,其中石墨化炉的温度加热至3200℃,冷却维护时长控制在286h。最后对石墨化品进行指标检测后再将其加工成规定规格的成品,而后按规定的匹配要求进行预组装、包装、入库。
上述获得的复合电极的指标检测结果如下表3和表4:
表3复合石墨电极的质量指标检测
表4复合石墨电极的质量指标检测
从表3和表4的测量结果可知,本发明制备的复合石墨电极的功率高,实用性强。
在本说明书的描述中,参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不一定指的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上显示和描述了本发明的基本原理、主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。
Claims (10)
1.一种复合石墨电极,其特征在于,所述制备原料按质量计如下:
25-35份石油焦、18-27份针状焦、9-13份煤沥青、3-8份的β-SiC、1-1.5份Fe2O3、0.6-0.9份脂肪醇聚氧乙烯醚、0.4-0.7份AL2O3、1-3份铜粉、2-4份Na2CO3;
所述复合石墨电极的指标如下:5.5uΩ·m≦电阻率≦6.5uΩ·m,1.62g/cm3≦体积密度≦1.66g/cm3,10.5MPa≦抗折强度≦11MPa,12GPa≦弹性模量≦14GPa,1.5×10-6m/℃≦热膨胀系数≦2.4×10-6m/℃。
2.根据权利要求1所述的一种复合石墨电极,其特征在于,所述制备原料按质量计如下:25份石油焦、18份针状焦、9份煤沥青、3份的β-SiC、1份Fe2O3、0.6份脂肪醇聚氧乙烯醚、0.4份AL2O3、1份铜粉、2份Na2CO3。
3.根据权利要求1所述的一种复合石墨电极,其特征在于,所述制备原料按质量计如下:30份石油焦、23份针状焦、11份煤沥青、6份β-SiC、1.2份Fe2O3、0.8份脂肪醇聚氧乙烯醚、0.6份AL2O3、2份铜粉、3份Na2CO3。
4.根据权利要求1所述的一种复合石墨电极,其特征在于,所述制备原料按质量计如下:35份石油焦、27份针状焦、13份煤沥青、8份的β-SiC、1.5份Fe2O3、0.9份脂肪醇聚氧乙烯醚、0.7份AL2O3、3份铜粉、4份Na2CO3。
5.一种复合石墨电极的制备方法,其特征在于,所述具体步骤如下所示:
步骤一,原料粉碎,称取石油焦、针状焦、煤沥青、β-SiC、Fe2O3、AL2O3、铜粉和Na2CO3后,再利用粉碎机分别将其粉碎成纳米级粉末;
步骤二,原料筛分,利用气流筛分机对步骤一中粉碎的石油焦、针状焦、煤沥青、β-SiC、Fe2O3、AL2O3、铜粉和Na2CO3粉末分别进行筛分获得8-15nm的原料粉末;
步骤三,物料干混,称取石油焦、针状焦、和β-SiC纳米级粉末放入混捏锅内搅拌混合均匀,再依次加入Fe2O3、AL2O3、AL2O3和Na2CO3纳米级粉末以及脂肪醇聚氧乙烯醚搅拌进行干混;
步骤四,物料混捏,混捏完成后获得糊料;
步骤五,物料成型,将糊料放入成型机内,利用20MPa的压力将其压制成石墨电极半成品;
步骤六,石墨电极半成品焙烧,将石墨电极半成品放入环式焙烧炉内按照设计的升温曲线对其进行焙烧,并在最高温度1500℃保持25h后自然降温,冷却78h后获得石墨电极焙烧品;
步骤七,石墨电极焙烧品石墨化处理,将焙烧品放入石墨化炉内,按送电曲线对焙烧品进行石墨化处理,在此过程中,石墨化炉的温度加热至2800-3200℃,冷却维护时长控制在255-286h;
步骤八,质量指标检测,对石墨化品的电阻率、体积密度、抗折强度、弹性模量和热膨胀系数进行检测以判定石墨电极的质量;
步骤九,将石墨化品加工成规定规格的成品,而后按规定的匹配要求进行预组装、包装、入库。
6.根据权利要求5所述的一种复合石墨电极的制备方法,其特征在于,所述步骤三中物料干混时混捏锅内搅拌器的搅拌速度为1200-1500r/min,干混时间为20-30min。
7.根据权利要求5所述的一种复合石墨电极的制备方法,其特征在于,所述步骤四中物料混捏时混捏锅内温度升高至200-210℃,混捏时长控制在25-30min。
8.根据权利要求5所述的一种复合石墨电极的制备方法,其特征在于,所述步骤五中,物料压制过程中成型机内温度为145-150℃,压制时长控制在3-3.5h。
9.根据权利要求5所述的一种复合石墨电极的制备方法,其特征在于,所述步骤六中的升温包括八个阶段,八个阶段分别处于如下温区内:150-200℃、200-250℃、250-450℃、450-600℃、600-800℃、800-1200℃、1200-1500℃、1500。
10.根据权利要求5所述的一种复合石墨电极的制备方法,其特征在于,所述步骤七送电曲线包括七个阶段,每个阶段的具体送电功率如下:2000KW、3000KW、4500KW、6500KW、8500KW、11500KW、13500KW。
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