CN110627518A - 一种高强度复合石墨电极的制备方法 - Google Patents
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Abstract
本发明一种高强度复合石墨电极的制备方法,涉及电极制备技术领域;具体是将制备原料粉碎成纳米级,并在反应釜中用乙醇气体进行活化反应,添加石墨烯纤维混捏后焙烧,之后浸入氯化银或氯化铜溶液进行离子吸附,吸附后干燥并石墨化处理;本发明在混捏成型之前对原料进行活化,有利于在形成石墨电极的过程中原料之间的结合力加强,提高石墨电极在使用时防折损率;本发明在增加石墨烯纤维和添加剂的基础上,结合原料前期的活化及半成品后期的离子吸附,有效提高了成品石墨电极的强度,使其具有更高的强度,同时具有高熔点和高弹性系数,良好的电热传导性,较小的热膨胀性能和较好的冲击性能。
Description
技术领域
本发明涉及电极制备技术领域,具体是一种高强度复合石墨电极的制备方法。
背景技术
石墨电极,主要以石油焦、针状焦为原料,煤沥青作结合剂,经煅烧、配料、混捏、压型、焙烧、石墨化、机加工而制成,是在电弧炉中以电弧形式释放电能对炉料进行加热熔化的导体,根据其质量指标高低,可分为普通功率、高功率和超高功率。
但是,目前的石墨电极由于结构不稳定,强度不高,在高温环境下很容易被氧化,因此石墨电极从氧化部位开始往下逐渐变细,使电极的抗耗性能下降,而石墨电极经过抗氧化处理后,又会一定程度的降低石墨电极的发射性能和产量,同时提高了生产周期和能耗。怎样提供一种结构稳定,强度高抗氧化性能强且安全可靠的石墨电极,是目前所要解决的问题。
发明内容
本发明克服现有技术存在的不足,提供一种高强度复合石墨电极的制备方法,目的是提高石墨电极的强度,解决由于石墨电极强度低造成的结构稳定性差,抗耗性能低的问题。
本发明是通过如下技术方案实现的。
一种高强度复合石墨电极的制备方法,包括以下具体步骤:
1)按照重量份称取原料:30-32份石油焦、20-25份针状焦、10-12份煤沥青、5-7份的β-SiC、0.5-0.7份脂肪醇聚氧乙烯醚、0.5-0.8份甲基萘磺酸钠、0.5-0.8份CaO、0.5-0.7份AL2O3、1-3份铜粉。
2)原料活化处理:将固体形态的各原料分别粉碎并筛分至粒径为30-50nm的粉末之后,将石油焦、针状焦、铜粉和β-SiC充分混合形成混合物A,将A放入反应釜,并在反应釜内通入A质量5-8%的乙醇气体,350-450℃下搅拌反应3-5h,得到反应物B。
3)物料成型:将B降温至100-150℃,加入脂肪醇聚氧乙烯醚、甲基萘磺酸钠、CaO和AL2O3充分混合后,加入煤沥青混合制成糊料,在糊料中加入石墨烯纤维继续混合,之后在成型机中混捏成型。
4)半成品焙烧:将混捏成型后得到的半成品进行焙烧,焙烧之后自然降温,放置72h之后得到石墨电极焙烧品。
5)离子吸附:将获得的石墨电极焙烧品完全浸没到离子溶液中静置48-72h,之后烘干,所述的离子溶液为浓度12-18mol/L的氯化银或氯化铜溶液。
6)石墨化处理:将干燥后的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3300-3500℃,冷却维护时长控制在300-320h,得到成品石墨电极。
优选的,所述步骤2中反应釜的反应压力为8-15MPa。
优选的,所述步骤2中将石油焦、针状焦、铜粉和β-SiC充分混合采用的搅拌速度为1500-1800r/min,混合时间为20-30min。
优选的,所述步骤3中加入的石墨烯纤维为糊料质量的6-10%,石墨烯纤维的直径为0.5-1mm。
优选的,所述步骤4中焙烧的温度为1200-1500℃。
优选的,所述的离子溶液为浓度16mol/L的氯化银溶液。
本发明相对于现有技术所产生的有益效果为。
本发明在混捏成型之前对原料进行活化,气态乙醇在一定温度及压力下对石油焦、针状焦表面的含氧基团进行清除,有利于在形成石墨电极的过程中原料之间的结合力加强。原料中加入甲基萘磺酸钠和CaO提高了石墨电极的抗氧化性能,提高石墨电极在使用时防折损率;在得到焙烧后的半成品,本发明增加离子吸附的步骤,使石墨电极内部的石墨烯纤维与其他原料之间形成的枝状结构上附着银或铜离子,有效提高石墨电极的导电性能,使其具有稳定的电流导通率。本发明在增加石墨烯纤维和添加剂的基础上,结合原料前期的活化及半成品后期的离子吸附,有效提高了成品石墨电极的强度,使其具有更高的强度,同时具有高熔点和高弹性系数,良好的电热传导性,同时具有较小的热膨胀性能和较好的冲击性能。
具体实施方式
为了使本发明所要解决的技术问题、技术方案及有益效果更加清楚明白,结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。下面结合实施例详细说明本发明的技术方案,但保护范围不被此限制。
实施例1
一种高强度复合石墨电极的制备方法,包括以下具体步骤:
1)称取原料:称取30kg的石油焦、23kg针状焦、10kg煤沥青、5kg β-SiC、0.7kg的脂肪醇聚氧乙烯醚、0.5kg的甲基萘磺酸钠、0.6kg的CaO、0.5kg的AL2O3、1kg的铜粉。
2)原料活化处理:将石油焦、针状焦、β-SiC、CaO、AL2O3和铜粉分别粉碎为纳米级的粉末,并使用气流筛分机将其筛分至粒径为30-50nm的粉末之后,将石油焦、针状焦、铜粉和β-SiC充分混合形成混合物A,混合采用的搅拌机的搅拌速度为1800r/min,混合时间为30min。将A放入超临界搅拌反应釜,并在反应釜内通入A质量6%的乙醇气体,12MPa、350℃下搅拌反应4h,得到反应物B。
3)物料成型:将B降温至120℃左右,加入脂肪醇聚氧乙烯醚、甲基萘磺酸钠、CaO和AL2O3充分混合后,加入煤沥青混合制成糊料,在糊料中加入其重量8%的石墨烯纤维继续混合,之后在成型机中混捏成型,其中石墨烯纤维的直径为0.5-1mm。
4)半成品焙烧:将混捏成型后得到的半成品进行焙烧,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1200℃保持20h后自然降温,冷却78h后获得石墨电极焙烧品。
5)离子吸附:将获得的石墨电极焙烧品完全浸没到浓度16mol/L的氯化银溶液中静置72h,之后烘干。
6)石墨化处理:将干燥后的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3500℃,冷却维护时长控制在320h,得到成品石墨电极。
7)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。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。
所制备的成品石墨电极的检测参数如下:
电阻率为5.5uΩ·m,体积密度为1.61g/cm3,抗折强度为12.3MPa,弹性模量15.8GPa,热膨胀系数为1.3×10-6m/℃。
实施例2
一种高强度复合石墨电极的制备方法,包括以下具体步骤:
1)称取原料:称取32kg的石油焦、20kg针状焦、11kg煤沥青、7kg β-SiC、0.5kg的脂肪醇聚氧乙烯醚、0.5kg的甲基萘磺酸钠、0.7kg的CaO、0.6kg的AL2O3、1.5kg的铜粉。
2)原料活化处理:将石油焦、针状焦、β-SiC、CaO、AL2O3和铜粉分别粉碎为纳米级的粉末,并使用气流筛分机将其筛分至粒径为30-50nm的粉末之后,将石油焦、针状焦、铜粉和β-SiC充分混合形成混合物A,混合采用的搅拌机的搅拌速度为1800r/min,混合时间为30min。将A放入超临界搅拌反应釜,并在反应釜内通入A质量8%的乙醇气体,10MPa、400℃下搅拌反应4.5h,得到反应物B。
3)物料成型:将B降温至150℃左右,加入脂肪醇聚氧乙烯醚、甲基萘磺酸钠、CaO和AL2O3充分混合后,加入煤沥青混合制成糊料,在糊料中加入其重量6%的石墨烯纤维继续混合,之后在成型机中混捏成型,其中石墨烯纤维的直径为0.5-1mm。
4)半成品焙烧:将混捏成型后得到的半成品进行焙烧,将石墨电极半成品放入环式焙烧炉内对其进行焙烧,并在最高温度1500℃保持20h后自然降温,冷却80h后获得石墨电极焙烧品。
5)离子吸附:将获得的石墨电极焙烧品完全浸没到浓度18mol/L的氯化银溶液中静置72h,之后烘干。
6)石墨化处理:将干燥后的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3300℃,冷却维护时长控制在320h,得到成品石墨电极。
7)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。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。
所制备的成品石墨电极的检测参数如下:
电阻率为5.3uΩ·m,体积密度为1.63g/cm3,抗折强度为12.9MPa,弹性模量15.7GPa,热膨胀系数为1.28×10-6m/℃。
实施例3
一种高强度复合石墨电极的制备方法,包括以下具体步骤:
1)称取原料:称取31kg的石油焦、25kg针状焦、12kg煤沥青、6kg β-SiC、0.6kg的脂肪醇聚氧乙烯醚、0.5kg的甲基萘磺酸钠、0.6kg的CaO、0.7kg的AL2O3、2kg的铜粉。
2)原料活化处理:将石油焦、针状焦、β-SiC、CaO、AL2O3和铜粉分别粉碎为纳米级的粉末,并使用气流筛分机将其筛分至粒径为30-50nm的粉末之后,将石油焦、针状焦、铜粉和β-SiC充分混合形成混合物A,混合采用的搅拌机的搅拌速度为1500r/min,混合时间为20min。将A放入超临界搅拌反应釜,并在反应釜内通入A质量5%的乙醇气体,15MPa、350℃下搅拌反应4h,得到反应物B。
3)物料成型:将B降温至130℃左右,加入脂肪醇聚氧乙烯醚、甲基萘磺酸钠、CaO和AL2O3充分混合后,加入煤沥青混合制成糊料,在糊料中加入其重量6%的石墨烯纤维继续混合,之后在成型机中混捏成型,其中石墨烯纤维的直径为0.5-1mm。
4)半成品焙烧:将混捏成型后得到的半成品进行焙烧,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1400℃保持20h后自然降温,冷却72h后获得石墨电极焙烧品。
5)离子吸附:将获得的石墨电极焙烧品完全浸没到浓度12mol/L的氯化铜溶液中静置72h,之后烘干。
6)石墨化处理:将干燥后的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3200℃,冷却维护时长控制在320h,得到成品石墨电极。
7)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。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。
所制备的成品石墨电极的检测参数如下:
电阻率为5.7uΩ·m,体积密度为1.60g/cm3,抗折强度为11.9MPa,弹性模量14.9GPa,热膨胀系数为1.21×10-6m/℃。
由以上是实施例证明,本发明在混捏成型之前对原料进行活化,气态乙醇在一定温度及压力下对石油焦、针状焦表面的含氧基团进行清除,有利于在形成石墨电极的过程中原料之间的结合力加强。原料中加入甲基萘磺酸钠和CaO提高了石墨电极的抗氧化性能,提高石墨电极在使用时防折损率;在得到焙烧后的半成品,本发明增加离子吸附的步骤,使石墨电极内部的石墨烯纤维与其他原料之间形成的枝状结构上附着银或铜离子,有效提高石墨电极的导电性能,使其具有稳定的电流导通率。本发明在增加石墨烯纤维和添加剂的基础上,结合原料前期的活化及半成品后期的离子吸附,有效提高了成品石墨电极的强度,使其具有更高的强度,同时具有高熔点和高弹性系数,良好的电热传导性,同时具有较小的热膨胀性能和较好的冲击性能。
以上内容是结合具体的优选实施方式对本发明所做的进一步详细说明,不能认定本发明的具体实施方式仅限于此,对于本发明所属技术领域的普通技术人员来说,在不脱离本发明的前提下,还可以做出若干简单的推演或替换,都应当视为属于本发明由所提交的权利要求书确定专利保护范围。
Claims (6)
1.一种高强度复合石墨电极的制备方法,其特征在于,包括以下具体步骤:
1)按照重量份称取原料:30-32份石油焦、20-25份针状焦、10-12份煤沥青、5-7份的β-SiC、0.5-0.7份脂肪醇聚氧乙烯醚、0.5-0.8份甲基萘磺酸钠、0.5-0.8份CaO、0.5-0.7份AL2O3、1-3份铜粉;
2)原料活化处理:将固体形态的各原料分别粉碎并筛分至粒径为30-50nm的粉末之后,将石油焦、针状焦、铜粉和β-SiC充分混合形成混合物A,将A放入反应釜,并在反应釜内通入A质量5-8%的乙醇气体,350-450℃下搅拌反应3-5h,得到反应物B;
3)物料成型:将B降温至100-150℃,加入脂肪醇聚氧乙烯醚、甲基萘磺酸钠、CaO和AL2O3充分混合后,加入煤沥青混合制成糊料,在糊料中加入石墨烯纤维继续混合,之后在成型机中混捏成型;
4)半成品焙烧:将混捏成型后得到的半成品进行焙烧,焙烧之后自然降温,放置72h之后得到石墨电极焙烧品;
5)离子吸附:将获得的石墨电极焙烧品完全浸没到离子溶液中静置48-72h,之后烘干,所述的离子溶液为浓度12-18mol/L的氯化银或氯化铜溶液;
6)石墨化处理:将干燥后的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3300-3500℃,冷却维护时长控制在300-320h,得到成品石墨电极。
2.根据权利要求1所述的一种高强度复合石墨电极的制备方法,其特征在于,所述步骤2中反应釜的反应压力为8-15MPa。
3.根据权利要求1所述的一种高强度复合石墨电极的制备方法,其特征在于,所述步骤2中将石油焦、针状焦、铜粉和β-SiC充分混合采用的搅拌速度为1500-1800r/min,混合时间为20-30min。
4.根据权利要求1所述的一种高强度复合石墨电极的制备方法,其特征在于,所述步骤3中加入的石墨烯纤维为糊料质量的6-10%,石墨烯纤维的直径为0.5-1mm。
5.据权利要求1所述的一种高强度复合石墨电极的制备方法,其特征在于,所述步骤4中焙烧的温度为1200-1500℃。
6.根据权利要求1所述的一种高强度复合石墨电极的制备方法,其特征在于,所述的离子溶液为浓度16mol/L的氯化银溶液。
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