CN108585858A - 一种复合石墨电极的制备工艺 - Google Patents
一种复合石墨电极的制备工艺 Download PDFInfo
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Abstract
本发明公开了一种复合石墨电极的制备工艺,包括如下步骤:S1、配料;S2、成型;S3、焙烧与浸渍;S4、石墨化,将S35处理后的原料放入内热串接(LWG)炉内,充入保护气体并加热至2700‑3000℃,保持15‑30小时,使其石墨化;S5、机加工,将S4处理后的原料进行机加工,直到达到预设尺寸,即制造出石墨电极。本发明工艺简单,且制造成本偏低,成品性能不弱于市场上的主流成品,甚至优于进口成品。因此,能够为企业带来更大的利润空间,提高企业的竞争力。
Description
技术领域
本发明涉及一种石墨电极,特别是涉及一种复合石墨电极的制备工艺。
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:
(1)用于电弧炼钢炉
电炉炼钢是石墨电极的使用大户。我国电炉钢产量约占粗钢产量的18%左右,炼钢用石墨电极占石墨电极总用量的70%~80%。电炉炼钢是利用石墨电极向炉内导入电流,利用电极端部和炉料之间引发电弧所产生的高温热源来进行冶炼。
(2)用于矿热电炉
矿热电炉主要用于生产工业硅和黄磷等,其特点是导电电极的下部埋在炉料中,在料层内形成电弧,并利用炉料自身的电阻所发出的热能来加热炉料,其中要求电流密度较高的矿热电炉需用石墨电极,例如每生产1t硅需消耗石墨电极约100kg,每生产1t黄磷需消耗石墨电极约40kg。
(3)用于电阻炉
生产石墨制品的石墨化炉、熔化玻璃的熔窑和生产碳化硅用的电炉等都属于电阻炉,炉内所装物料既是发热电阻又是被加热对象,通常,导电用的石墨电极嵌入电阻炉端部的炉头墙中,用于此处的石墨电极不连续消耗。
(4)用于制备异型石墨产品
石墨电极的毛坯还用于加工成各种坩埚、模具、舟皿和发热体等异型石墨产品。例如,在石英玻璃行业,每生产1t电熔管,需用石墨电极坯料10t;每生产1t石英砖,需消耗石墨电极坯料100kg。
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。
因此,申请人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
有鉴于现有技术的上述缺陷,本发明所要解决的技术问题是提供一种复合石墨电极的制备工艺。
为实现上述目的,本发明提供了一种复合石墨电极的制备工艺,包括如下步骤:
S1、配料
S11、原料,石油焦、针状焦、煤沥青、碳纳米管、铜粉、二硫化钼、腐植酸,所述的铜粉纯度为99.9%以上、细度为100-120目;腐植酸细度为100-120目;所述的煤沥青的软化点为90-100℃,结焦值为≥55%,灰分≤0.20%;
S12、将石油焦、针状焦放入煅烧炉中,通入保护气(氩气),然后加热到1250-1350℃,保持0.5-1小时,进行煅烧;
S13、将S12中煅烧后的石油焦、针状焦进行破碎、细磨,使其粒径不大于0.075㎜;
S14、将以下组分按照重量份数比均匀混合,S13处理后的石油焦10-12、S13处理后的针状焦4-8、碳纳米管1-2、铜粉1-3、二硫化钼0.5-1、腐植酸0.5-1。混合时可以加入无水乙醇进行湿混,混合完成后烘干,从而提高其混合效率;
S15、将按照以下组分重量份数比取出并均匀混合,S14中混合的原料5-6、煤沥青3-4,混合时间1-2小时;
S2、成型
S21、将S15处理后的原料进行搅拌,且将原料温度增加到90-120℃,搅拌1-2小时;
S22、将S21中混合后的原料放入压力机中通过4-10MPa压实;
S23、将S22中压实的原料通过20-25MPa的压力压紧,保持3-5min,同时抽真空;
S24、将S23中处理后的原料放入挤压机中,加热至100-150℃,通过5-15MPa的压力进行挤压,然后按照预设要求剪切成段,在剪切成段的前,向挤压出来的材料喷射温度为10-25℃的水雾,以使其快速降温;
S3、焙烧与浸渍
S31、一次焙烧,将S24中切断的原料放入焙烧炉中,通过1000-1250℃高温进行焙烧,且充入保护气(氩气);
中升温方式如下:
0-400℃,10℃/min,达到400℃后保持1-2小时;
401-800℃,15℃/min,达到800℃后保持1-2小时;
801-1250℃,25℃/min;达到1250℃后保持320-480小时;
焙烧完成后,停止加热,自然冷却至800℃,然后取出风冷至室温;
S32、浸渍,将S31处理后的原料进行表面清理,然后放入浸渍罐内,并预热至300-450℃,保持6-8小时;
然后将浸渍罐抽真空,并保持1-2小时,再将煤沥青加热至250-300℃后注入浸渍罐内使得原料完全浸入煤沥青内;
然后,往浸渍罐内加入保护气,直到气压达到10-15MPa后,保持8-12小时;
最后泄压,排出煤沥青,原料在浸渍罐内冷却至室温,取出并清理表面;
S33、二次焙烧,将S32处理后的原料再次放入焙烧炉内,通过850-900℃高温进行再次焙烧,且充入保护气;
升温方式如下:
0-400℃,20℃/min;
401-900℃,40℃/min,达到800℃后保持250-320小时,然后在焙烧炉内冷却至室温,取出清理表面。
S34、重复S32-S33两次以上,每次检查浸渍原料的浸渍增重率;
检查的具体标准如下:
浸渍增重率G=(W2-W1)/W1×100% ;W1为浸渍前重量,W2为浸渍后重量;
一次浸渍品增重率≥14%;
二次浸渍品增重率≥9%;
三次浸渍品增重率≥5%;
S35、在焙烧炉内装入钢碳,然后将S34处理后的原料放入钢碳中,充入保护气,气压为2-6KPa,然后加热至900-1000℃,保持2-4小时;
S4、石墨化,将S35处理后的原料放入内热串接(LWG)炉内,充入保护气体并加热至2700-3000℃,保持15-30小时,使其石墨化;
升温方式如下:
0-400℃,20℃/min;
401-800℃,30℃/min;
801-1500℃,50℃/min;
1501-3000℃,80℃/min;
S5、机加工,将S4处理后的原料进行机加工,直到达到预设尺寸,即制造出石墨电极。
本发明的有益效果是:本发明工艺简单,且制造成本偏低,成品性能不弱于市场上的主流成品,甚至优于进口成品。因此,能够为企业带来更大的利润空间,提高企业的竞争力。
本发明在原料中加入了铜粉,可有效提高产品的耐电腐蚀性和强度。同时不会影响整个石墨电极的正常性能。
具体实施方式
下面结合实施例对本发明作进一步说明:
实施例一
一种复合石墨电极的制备工艺,包括如下步骤:
S1、配料
S11、原料,石油焦、针状焦、煤沥青、碳纳米管、铜粉、二硫化钼、腐植酸,所述的铜粉纯度为99.9%以上、细度为100-120目;腐植酸细度为100-120目;所述的煤沥青的软化点为90-100℃,结焦值为≥55%,灰分≤0.20%;
S12、将石油焦、针状焦放入煅烧炉中,通入保护气(氩气),然后加热到1250-1350℃,保持0.5-1小时,进行煅烧;
S13、将S12中煅烧后的石油焦、针状焦进行破碎、细磨,使其粒径不大于0.075㎜;
S14、将以下组分按照重量份数比均匀混合,S13处理后的石油焦12、S13处理后的针状焦8、碳纳米管1.5、铜粉1、二硫化钼0.6、腐植酸0.5。混合时可以加入无水乙醇进行湿混,混合完成后烘干,从而提高其混合效率;
S15、将按照以下组分重量份数比取出并均匀混合,S14中混合的原料5.5、煤沥青4,混合时间1-2小时;
S2、成型
S21、将S15处理后的原料进行搅拌,且将原料温度增加到100℃,搅拌1-2小时;
S22、将S21中混合后的原料放入压力机中通过10MPa压实;
S23、将S22中压实的原料通过25MPa的压力压紧,保持3-5min,同时抽真空;
S24、将S23中处理后的原料放入挤压机中,加热至130℃,通过15MPa的压力进行挤压,然后按照预设要求剪切成段,在剪切成段的前,向挤压出来的材料喷射温度为10-25℃的水雾,以使其快速降温;
S3、焙烧与浸渍
S31、一次焙烧,将S24中切断的原料放入焙烧炉中,通过1250℃高温进行焙烧,且充入保护气(氩气);
中升温方式如下:
0-400℃,10℃/min,达到400℃后保持1-2小时;
401-800℃,15℃/min,达到800℃后保持1-2小时;
801-1250℃,25℃/min;达到1250℃后保持320-480小时;
焙烧完成后,停止加热,自然冷却至800℃,然后取出风冷至室温;
S32、浸渍,将S31处理后的原料进行表面清理,然后放入浸渍罐内,并预热至450℃,保持6-8小时;
然后将浸渍罐抽真空,并保持1-2小时,再将煤沥青加热至250-300℃后注入浸渍罐内使得原料完全浸入煤沥青内;
然后,往浸渍罐内加入保护气,直到气压达到15MPa后,保持10小时;
最后泄压,排出煤沥青,原料在浸渍罐内冷却至室温,取出并清理表面;
S33、二次焙烧,将S32处理后的原料再次放入焙烧炉内,通过900℃高温进行再次焙烧,且充入保护气;
升温方式如下:
0-400℃,20℃/min;
401-900℃,40℃/min,达到800℃后保持320小时,然后在焙烧炉内冷却至室温,取出清理表面。
S34、重复S32-S33两次以上,每次检查浸渍原料的浸渍增重率;
检查的具体标准如下:
浸渍增重率G=(W2-W1)/W1×100% ;W1为浸渍前重量,W2为浸渍后重量;
一次浸渍品增重率≥14% ;
二次浸渍品增重率≥9% ;
三次浸渍品增重率≥5%;
S35、在焙烧炉内装入钢碳,然后将S34处理后的原料放入钢碳中,充入保护气,气压为2-6KPa,然后加热至1000℃,保持2-4小时;
S4、石墨化,将S35处理后的原料放入内热串接(LWG)炉内,充入保护气体并加热至2800℃,保持20小时,使其石墨化;
升温方式如下:
0-400℃,20℃/min;
401-800℃,30℃/min;
801-1500℃,50℃/min;
1501-3000℃,80℃/min;
S5、机加工,将S4处理后的原料进行机加工,直到达到预设尺寸,即制造出石墨电极。
实施例二
一种复合石墨电极的制备工艺,包括如下步骤:
S1、配料
S11、原料,石油焦、针状焦、煤沥青、碳纳米管、铜粉、二硫化钼、腐植酸,所述的铜粉纯度为99.9%以上、细度为100-120目;腐植酸细度为100-120目;所述的煤沥青的软化点为90-100℃,结焦值为≥55%,灰分≤0.20%;
S12、将石油焦、针状焦放入煅烧炉中,通入保护气(氩气),然后加热到1350℃,保持0.5-1小时,进行煅烧;
S13、将S12中煅烧后的石油焦、针状焦进行破碎、细磨,使其粒径不大于0.075㎜;
S14、将以下组分按照重量份数比均匀混合,S13处理后的石油焦11、S13处理后的针状焦6、碳纳米管1.2、铜粉1.2、二硫化钼0.6、腐植酸0.5。混合时可以加入无水乙醇进行湿混,混合完成后烘干,从而提高其混合效率;
S15、将按照以下组分重量份数比取出并均匀混合,S14中混合的原料5-6、煤沥青3.2,混合时间1-2小时;
S2、成型
S21、将S15处理后的原料进行搅拌,且将原料温度增加到90-120℃,搅拌1-2小时;
S22、将S21中混合后的原料放入压力机中通过8MPa压实;
S23、将S22中压实的原料通过25MPa的压力压紧,保持3-5min,同时抽真空;
S24、将S23中处理后的原料放入挤压机中,加热至100-150℃,通过10MPa的压力进行挤压,然后按照预设要求剪切成段,在剪切成段的前,向挤压出来的材料喷射温度为20℃的水雾,以使其快速降温;
S3、焙烧与浸渍
S31、一次焙烧,将S24中切断的原料放入焙烧炉中,通过1250℃高温进行焙烧,且充入保护气(氩气);
中升温方式如下:
0-400℃,10℃/min,达到400℃后保持1-2小时;
401-800℃,15℃/min,达到800℃后保持1-2小时;
801-1250℃,25℃/min;达到1250℃后保持450小时;
焙烧完成后,停止加热,自然冷却至800℃,然后取出风冷至室温;
S32、浸渍,将S31处理后的原料进行表面清理,然后放入浸渍罐内,并预热至400℃,保持6-8小时;
然后将浸渍罐抽真空,并保持1-2小时,再将煤沥青加热至300℃后注入浸渍罐内使得原料完全浸入煤沥青内;
然后,往浸渍罐内加入保护气,直到气压达到10-15MPa后,保持8-12小时;
最后泄压,排出煤沥青,原料在浸渍罐内冷却至室温,取出并清理表面;
S33、二次焙烧,将S32处理后的原料再次放入焙烧炉内,通过850-900℃高温进行再次焙烧,且充入保护气;
升温方式如下:
0-400℃,20℃/min;
401-900℃,40℃/min,达到800℃后保持300小时,然后在焙烧炉内冷却至室温,取出清理表面。
S34、重复S32-S33两次以上,每次检查浸渍原料的浸渍增重率;
检查的具体标准如下:
浸渍增重率G=(W2-W1)/W1×100% ;W1为浸渍前重量,W2为浸渍后重量;
一次浸渍品增重率≥14% ;
二次浸渍品增重率≥9% ;
三次浸渍品增重率≥5%;
S35、在焙烧炉内装入钢碳,然后将S34处理后的原料放入钢碳中,充入保护气,气压为2-6KPa,然后加热至950℃,保持2-4小时;这种方式主要是增加原料表面的含碳量。
S4、石墨化,将S35处理后的原料放入内热串接(LWG)炉内,充入保护气体并加热至3000℃,保持25小时,使其石墨化;
升温方式如下:
0-400℃,20℃/min;
401-800℃,30℃/min;
801-1500℃,50℃/min;
1501-3000℃,80℃/min;
S5、机加工,将S4处理后的原料进行机加工,直到达到预设尺寸,即制造出石墨电极。
本发明未详述之处,均为本领域技术人员的公知技术。
以上详细描述了本发明的较佳具体实施例。应当理解,本领域的普通技术人员无需创造性劳动就可以根据本发明的构思作出诸多修改和变化。因此,凡本技术领域中技术人员依本发明的构思在现有技术的基础上通过逻辑分析、推理或者有限的实验可以得到的技术方案,皆应在由权利要求书所确定的保护范围内。
Claims (6)
1.一种复合石墨电极的制备工艺,其特征在于,包括如下步骤:
S1、配料
S11、原料,石油焦、针状焦、煤沥青、碳纳米管、铜粉、二硫化钼、腐植酸,所述的铜粉纯度为99.9%以上、细度为100-120目;腐植酸细度为100-120目;所述的煤沥青的软化点为90-100℃,结焦值为≥55%,灰分≤0.20%;
S12、将石油焦、针状焦放入煅烧炉中,通入保护气,然后加热到1250-1350℃,保持0.5-1小时,进行煅烧;
S13、将S12中煅烧后的石油焦、针状焦进行破碎、细磨,使其粒径不大于0.075㎜;
S14、将以下组分按照重量份数比均匀混合,S13处理后的石油焦10-12、S13处理后的针状焦4-8、碳纳米管1-2、铜粉1-3、二硫化钼0.5-1、腐植酸0.5-1;
S15、将按照以下组分重量份数比取出并均匀混合,S14中混合的原料5-6、煤沥青3-4,混合时间1-2小时;
S2、成型
S21、将S15处理后的原料进行搅拌,且将原料温度增加到90-120℃,搅拌1-2小时;
S22、将S21中混合后的原料放入压力机中通过4-10MPa压实;
S23、将S22中压实的原料通过20-25MPa的压力压紧,保持3-5min,同时抽真空;
S24、将S23中处理后的原料放入挤压机中,加热至100-150℃,通过5-15MPa的压力进行挤压,然后按照预设要求剪切成段;
S3、焙烧与浸渍
S31、一次焙烧,将S24中切断的原料放入焙烧炉中,通过1000-1250℃高温进行焙烧,且充入保护气;
S32、浸渍,将S31处理后的原料进行表面清理,然后放入浸渍罐内,并预热至300-450℃,保持6-8小时;
然后将浸渍罐抽真空,并保持1-2小时,再将煤沥青加热至250-300℃后注入浸渍罐内使得原料完全浸入煤沥青内;
然后,往浸渍罐内加入保护气,直到气压达到10-15MPa后,保持8-12小时;
最后泄压,排出煤沥青,原料在浸渍罐内冷却至室温,取出并清理表面;
S33、二次焙烧,将S32处理后的原料再次放入焙烧炉内,通过850-900℃高温进行再次焙烧,且充入保护气;
S34、重复S32-S33两次以上,每次检查浸渍原料的浸渍增重率;
S35、在焙烧炉内装入钢碳,然后将S34处理后的原料放入钢碳中,充入保护气,气压为2-6KPa,然后加热至900-1000℃,保持2-4小时;
S4、石墨化,将S35处理后的原料放入内热串接(LWG)炉内,充入保护气体并加热至2700-3000℃,保持15-30小时,使其石墨化;
S5、机加工,将S4处理后的原料进行机加工,直到达到预设尺寸,即制造出石墨电极。
2.如权利要求1所述的,其特征是:S24中,在剪切成段的前,向挤压出来的材料喷射温度为10-25℃的水雾。
3.如权利要求1所述的,其特征是:S31中升温方式如下:
0-400℃,10℃/min,达到400℃后保持1-2小时;
401-800℃,15℃/min,达到800℃后保持1-2小时;
801-1250℃,25℃/min;达到1250℃后保持320-480小时;
焙烧完成后,停止加热,自然冷却至800℃,然后取出风冷至室温。
4.如权利要求1所述的,其特征是:S33中升温方式如下:
0-400℃,20℃/min;
401-900℃,40℃/min,达到800℃后保持250-320小时,然后在焙烧炉内冷却至室温,取出清理表面。
5.如权利要求1所述的,其特征是:S34中检查的具体标准如下:
浸渍增重率G=(W2-W1)/W1×100% ;W1为浸渍前重量,W2为浸渍后重量;
一次浸渍品增重率≥14%;
二次浸渍品增重率≥9%;
三次浸渍品增重率≥5%。
6.如权利要求1所述的,其特征是:S4中升温方式如下:
0-400℃,20℃/min;
401-800℃,30℃/min;
801-1500℃,50℃/min;
1501-3000℃,80℃/min。
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