CN108863370B - 高强度石墨材料的制备工艺 - Google Patents
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Abstract
本发明涉及石墨材料制备领域,尤其涉及一种高强度石墨材料的制备工艺,包括以下步骤:选取生石油焦,将生石油焦投入滚筒炉中;制定升温曲线进行加热处理得到半焦,其中升温曲线的升温上限为500‑600℃;将半焦磨粉至平均粒度为5‑6μm,然后投入混捏锅中并向混捏锅中加入分散剂,升温至140‑150℃,混捏45‑50min,再向混捏锅内投入熔融粘结剂,保持温度140‑150℃,混捏45‑50min,得到糊料;将糊料经过2次轧片处理,得到轧片;将轧片磨粉至平均粒度为20‑22μm,然后成型得到生坯;将生坯进行焙烧,然后进行石墨化,得到成品高强度石墨材料,生产周期短、制作成本低、所得高强度石墨材料性能高。
Description
技术领域
本发明涉及石墨材料制备领域,尤其涉及一种高强度石墨材料的制备工艺。
背景技术
随着工业和高科技的发展,石墨材料自身的润滑性导电导热耐腐蚀性高温机械强度,被广泛用到磨具行业,半导体行业光伏电火花等行业,目前,传统的生产石墨制品的原料是煅后石油焦、煅后沥青焦,将煅后焦磨成20微米的粉,在加热的混捏锅中混60分钟,使粉料温度在150-160度,然后加入粘结剂是煤沥青,在混捏锅中混60分钟,使粉料和沥青搅拌均匀,然后混料经过轧片机轧片,然后磨粉,再成型和焙烧,生产出的产品因为体密和强度低,气孔率高,无法满足市场的需要,传统上为弥补产品的不足,需要通过数次浸渍和焙烧,才能满足市场的需要,但是这样生产周期长达7-8个月,生产成本增加。
发明内容
本发明的目的在于克服现有技术中的不足,提供一种生产周期短、制作成本低、所得高强度石墨材料性能高的高强度石墨材料的制备工艺。
本发明是通过以下技术方案实现的:一种高强度石墨材料的制备工艺,包括以下步骤:
步骤一,选取生石油焦,将生石油焦投入滚筒炉中;
步骤二,制定升温曲线进行加热处理得到半焦,其中升温曲线的升温上限为500-600℃;
步骤三,将步骤二得到的半焦磨粉至平均粒度为5-6μm,然后投入混捏锅中并向混捏锅中加入分散剂,升温至140-150℃,混捏45-50min,再向混捏锅内投入熔融粘结剂,保持温度140-150℃,混捏45-50min,得到一次糊料;
步骤四,将一次糊料经过2次轧片处理,得到厚度值为1.5-1.7mm的轧片;
步骤五,将轧片磨粉至平均粒度为20-22μm,然后成型得到生坯;
步骤六,将生坯进行焙烧,然后进行石墨化,得到成品高强度石墨材料,
生石油焦、高温改性沥青、聚乙烯蜡三者的重量比为55-60:35-39:0.3-0.6。
进一步地,步骤一中的生石油焦为抚顺生石油焦。
进一步地,步骤二中的制定升温曲线进行加热处理,升温上限为550℃,包括以下步骤:
A,经过30min将温度自室温均匀升温到50℃;
B,再经过30min将温度自50℃均匀升温到120℃;
C,再经过100min将温度自120℃均匀升温到240℃;
D,再经过40min将温度自240℃均匀升温到300℃;
E,再经过60min将温度自300℃均匀升温到350℃;
F,再经过40min将温度自350℃均匀升温到380℃;
G,再经过30min将温度自380℃均匀升温到410℃;
H,再经过30min将温度自410℃均匀升温到450℃;
I,再经过30min将温度自450℃均匀升温到480℃;
J,再经过30min将温度自480℃均匀升温到520℃;
K,再经过30min将温度自520℃均匀升温到550℃,持续120-150min。
进一步地,所述分散剂选用聚乙烯蜡。
进一步地,所述粘结剂为高温改制沥青。
进一步地,步骤三和步骤五中的磨粉均选用气流磨磨粉。
进一步地,在步骤二中向滚桶炉中通入用于防止生石油焦燃烧的保护气体。
进一步地,所述保护气体选用氩气或者氮气。
本发明的有益效果在于:选用抚顺生石油焦,低灰分低硫强度高,将生石油焦通过滚筒炉做升温上限为500-600℃的处理,能够得到收缩性大、挥发分含量高的半焦,半焦在焙烧和石墨化的过程中收缩,进而得到高真密度的石墨材料,制备成本低、周期短。
具体实施方式
以下各实施例中,生石油焦选用抚顺生石油焦,具体为抚顺石化二厂,1#A型生石油焦,生石油焦的灰分含量为0.12-0.18wt%、挥发分含量为10-15wt%,硫元素含量为0.23-0.27wt%,水分含量为6-8wt%,灰分低、硫元素含量低、强度高;
步骤二中升温曲线的升温上限为550℃,能够排出生焦中的小分子碳氢化合物以及水分,且能够提高生焦自身的强度、收缩性能及结焦值,所得半焦中灰分含量为0.09-0.13wt%、挥发分含量为5-8wt%,硫元素含量为0.18-0.21wt%,水分含量不大于0.01wt%,具体的升温曲线为:
A,经过30min将温度自室温均匀升温到50℃;
B,再经过30min将温度自50℃均匀升温到120℃;
C,再经过100min将温度自120℃均匀升温到240℃;
D,再经过40min将温度自240℃均匀升温到300℃;
E,再经过60min将温度自300℃均匀升温到350℃;
F,再经过40min将温度自350℃均匀升温到380℃;
G,再经过30min将温度自380℃均匀升温到410℃;
H,再经过30min将温度自410℃均匀升温到450℃;
I,再经过30min将温度自450℃均匀升温到480℃;
J,再经过30min将温度自480℃均匀升温到520℃;
K,再经过30min将温度自520℃均匀升温到550℃,持续150min。
粘结剂为高温改性沥青,高温改性沥青为宝钢梅山化工股份有限公司产品,该高温改性沥青灰分含量0.09wt%,挥发份含量52.3wt%,结焦值62.1%,甲苯不溶物含量32.8wt%。
分散剂具体为聚乙烯蜡,能够使粉料分散均匀,分散剂是高分子碳氢化合物,不影响产品质量。
步骤二中向滚桶炉中通入用于防止生石油焦燃烧的保护气体,保护气体选用氩气或者氮气,能够隔绝氧气、防止温度过高后焦自然或氧化,保护气体流速为1-1.5M3/H。
步骤四中,2次轧片为通过轧片机轧片两次,第一次轧片至2.5mm,第二次轧片至1.5-1.7mm,得到轧片。
步骤五中,成型是将粉料经2000t的压力等静压成型。
步骤六中,焙烧温度为1250-1300℃,石墨化温度为2900-3000℃。
实施例1
一种高强度石墨材料的制备工艺,包括以下步骤:
步骤一,选取生石油焦,将生石油焦投入滚筒炉中;
步骤二,制定升温曲线进行加热处理得到半焦,其中升温曲线的升温上限为550℃;
步骤三,将步骤二得到的半焦磨粉至平均粒度为5μm,然后投入混捏锅中并向混捏锅中加入分散剂,升温至140℃,混捏45min,再向混捏锅内投入熔融粘结剂,保持温度140℃,混捏45min,得到一次糊料;
步骤四,将一次糊料经过2次轧片处理,得到轧片;
步骤五,将轧片磨粉至平均粒度为20μm,然后成型得到生坯;
步骤六,将生坯进行焙烧,然后进行石墨化,得到成品高强度石墨材料,
生石油焦、高温改性沥青、聚乙烯蜡三者的重量分别为55kg、36kg、0.4kg。
所得高强度石墨材料理化性能见附表1。
实施例2
一种高强度石墨材料的制备工艺,包括以下步骤:
步骤一,选取生石油焦,将生石油焦投入滚筒炉中;
步骤二,制定升温曲线进行加热处理得到半焦,其中升温曲线的升温上限为550℃;
步骤三,将步骤二得到的半焦磨粉至平均粒度为6μm,然后投入混捏锅中并向混捏锅中加入分散剂,升温至145℃,混捏45min,再向混捏锅内投入熔融粘结剂,保持温度150℃,混捏45min,得到一次糊料;
步骤四,将一次糊料经过2次轧片处理,得到轧片;
步骤五,将轧片磨粉至平均粒度为22μm,然后成型得到生坯;
步骤六,将生坯进行焙烧,然后进行石墨化,得到成品高强度石墨材料,
生石油焦、高温改性沥青、聚乙烯蜡三者的重量分别为58kg、39kg、0.5kg。
所得高强度石墨材料理化性能见附表1。
实施例3
一种高强度石墨材料的制备工艺,包括以下步骤:
步骤一,选取生石油焦,将生石油焦投入滚筒炉中;
步骤二,制定升温曲线进行加热处理得到半焦,其中升温曲线的升温上限为550℃;
步骤三,将步骤二得到的半焦磨粉至平均粒度为5μm,然后投入混捏锅中并向混捏锅中加入分散剂,升温至150℃,混捏45min,再向混捏锅内投入熔融粘结剂,保持温度140℃,混捏45min,得到一次糊料;
步骤四,将一次糊料经过2次轧片处理,得到轧片;
步骤五,将轧片磨粉至平均粒度为21μm,然后成型得到生坯;
步骤六,将生坯进行焙烧,然后进行石墨化,得到成品高强度石墨材料,
生石油焦、高温改性沥青、聚乙烯蜡三者的重量分别为60kg、39.7kg、0.3kg。
所得高强度石墨材料理化性能见附表1。
实施例4
一种高强度石墨材料的制备工艺,包括以下步骤:
步骤一,选取生石油焦,将生石油焦投入滚筒炉中;
步骤二,制定升温曲线进行加热处理得到半焦,其中升温曲线的升温上限为550℃;
步骤三,将步骤二得到的半焦磨粉至平均粒度为6μm,然后投入混捏锅中并向混捏锅中加入分散剂,升温至150℃,混捏45min,再向混捏锅内投入熔融粘结剂,保持温度146℃,混捏45min,得到一次糊料;
步骤四,将一次糊料经过2次轧片处理,得到轧片;
步骤五,将轧片磨粉至平均粒度为20μm,然后成型得到生坯;
步骤六,将生坯进行焙烧,然后进行石墨化,得到成品高强度石墨材料,
生石油焦、高温改性沥青、聚乙烯蜡三者的重量分别为58kg、35kg、0.5kg。
所得高强度石墨材料理化性能见附表1。
附表1
本发明中,以石油焦为原料,通过滚筒炉升温在500-600℃的温度,自制出一种半焦状态下,自身仍然具备很大的收缩性,并且挥发份仍然在5%-8%,通过气流磨磨出6-9微米的超细粉,在混捏过程中,加入聚乙烯蜡做分散剂,使粉料均匀分散,混合高温改性沥青搅拌,轧片后再次磨出20微米的糊料粉,再等静压压制成型,通过一次焙烧利用自制焦较大的自收缩性,且半焦自身存在挥发份,降低了高温改制沥青的使用量,生产出高体密的碳材料,聚乙烯蜡成分是高分子碳氢化合物,在高温状态下通过化学反应增强的产品的强度,能够有效的降低生产周期,且制得的石墨产品抗压、抗折强度高、硬度高,适用于高精密部件的加工和电火花行业。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (3)
1.一种高强度石墨材料的制备工艺,其特征在于,包括以下步骤:
步骤一,选取生石油焦,将生石油焦投入滚筒炉中;
步骤二,制定升温曲线进行加热处理得到半焦,其中升温曲线的升温上限为500-600℃;
步骤三,将步骤二得到的半焦磨粉至平均粒度为5-6μm,然后投入混捏锅中并向混捏锅中加入分散剂,升温至140-150℃,混捏45-50min,再向混捏锅内投入熔融粘结剂,保持温度140-150℃,混捏45-50min,得到一次糊料;
步骤四,将一次糊料经过2次轧片处理,得到厚度值为1.5-1.7mm的轧片;
步骤五,将轧片磨粉至平均粒度为20-22μm,然后成型得到生坯;
步骤六,将生坯进行焙烧,然后进行石墨化,得到成品高强度石墨材料,
所述分散剂选用聚乙烯蜡,所述粘结剂为高温改质沥青,
所得半焦中灰分含量为0.09-0.13wt%、挥发分含量为5-8wt%,硫元素含量为0.18-0.21wt%,水分含量不大于0.01wt%,
高温改质沥青灰分含量0.09wt% ,挥发份含量52.3wt%,结焦值62.1%,甲苯不溶物含量32 .8wt%,
生石油焦、高温改质沥青、聚乙烯蜡三者的重量比为55-60:35-39:0.3-0.6,
步骤一中的生石油焦为抚顺生石油焦,生石油焦的灰分含量为0.12-0.18wt%、挥发分含量为10-15wt%,硫元素含量为0.23-0.27wt%,水分含量为6-8wt%,
步骤二中的制定升温曲线进行加热处理,升温上限为550℃,包括以下步骤:
A,经过30min将温度自室温均匀升温到50℃;
B,再经过30min将温度自50℃均匀升温到120℃;
C,再经过100min将温度自120℃均匀升温到240℃;
D,再经过40min将温度自240℃均匀升温到300℃;
E,再经过60min将温度自300℃均匀升温到350℃;
F,再经过40min将温度自350℃均匀升温到380℃;
G,再经过30min将温度自380℃均匀升温到410℃;
H,再经过30min将温度自410℃均匀升温到450℃;
I,再经过30min将温度自450℃均匀升温到480℃;
J,再经过30min将温度自480℃均匀升温到520℃;
K,再经过30min将温度自520℃均匀升温到550℃,持续150min,
步骤三和步骤五中的磨粉均选用气流磨磨粉。
2.根据权利要求1所述的高强度石墨材料的制备工艺,其特征在于,在步骤二中向滚桶炉中通入用于防止生石油焦燃烧的保护气体。
3.根据权利要求2所述的高强度石墨材料的制备工艺,其特征在于,所述保护气体选用氩气或者氮气。
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Denomination of invention: Preparation process of high-strength graphite material Granted publication date: 20210709 Pledgee: Industrial and Commercial Bank of China Pingdingshan Huaying Branch Pledgor: PINGDINGSHAN ORIENTAL CARBON Co.,Ltd. Registration number: Y2024980037764 |