CN116409993B - 一种高强度的中粗石墨的制备方法 - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 101
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Abstract
本发明公开了一种高强度的中粗石墨的制备方法，包括以下步骤：S1、将锻后的石墨焦研磨至干粉状；S2、选金属原料放入熔炉内，将温度逐渐加热至1100‑1200℃，使其均匀充分混合，混合后获得混合物；S3、向步骤2中获得的混合物内加入乙醇溶液，搅拌使其均匀分散，然后再进行低温冷冻处理，得到改性石墨凝胶体；S4、将改性石墨凝胶体依次经过混捏‑冷却成型‑石墨化工艺后，加工获得中粗石墨。本发明金属原料可以提高石墨的韧性，锆的耐腐蚀性比钛好、钛重量轻、强度高、具金属光泽，耐湿氯气腐蚀、铝质地坚韧而轻，有延展性，容易导电，还可增强石墨的导电性。
Description
技术领域
本发明涉及石墨技术领域，尤其涉及一种高强度的中粗石墨的制备方法。
背景技术
石墨是碳的一种同素异形体，为灰黑色、不透明固体，化学性质稳定，耐腐蚀，同酸、碱等药剂不易发生反应。天然石墨来自石墨矿藏，也可以以石油焦、沥青焦等为原料，经过一系列工序处理而制成人造石墨。石墨在氧气中燃烧生成二氧化碳，可被强氧化剂如浓硝酸、高锰酸钾等氧化。可用作抗磨剂、润滑剂，高纯度石墨用作原子反应堆中的中子减速剂，还可用于制造坩埚、电极、电刷、干电池、石墨纤维、换热器、冷却器、电弧炉、弧光灯、铅笔的笔芯等。
石墨还可制取散热材料、密封材料、隔热材料、和防辐射材料等，石墨功能材料广泛应用于冶金、化工、机械设备、新能源汽车、核电、电子信息、航空航天和国防等行业。欧盟委员会发布的《对欧盟生死攸关的原料》报告中，将石墨列入14种紧缺矿产原料，但石墨的本身弯曲强度和韧性不好，因此，需要提高石墨的韧性。
发明内容
本发明为了解决现有技术的上述不足，提出了一种高强度的中粗石墨的制备方法。
为了解决上述技术问题，本发明采用以下技术方案：一种高强度的中粗石墨的制备方法，包括以下步骤：
S1、将锻后的石墨焦研磨至干粉状，锻后焦粒含量为60-63％，焦粒粒度为0.4-0.6mm，煅后的焦粉含量为的含量为35-38％，焦粉的粒度为0.065-0.075mm；
S2、选金属原料放入熔炉内，金属原料与石墨焦的质量比为1:12，先预热只100-150℃，预热时间为10-15min，预热后，将温度逐渐加热至1100-1200℃，加热时间为0.5-1.1h，加热后保温30-35min，随后再向熔炉内加入步骤S1获得的石墨焦干粉继续加热30min，随后搅拌，使其均匀充分混合，混合后获得混合物；
S3、向步骤2中获得的混合物内加入乙醇溶液，该乙醇溶液的浓度为65％。在搅拌速度为1500-4000rpm的条件下搅拌15～20min使其均匀分散，然后再进行低温冷冻处理，得到改性石墨凝胶体；
S4、将改性石墨凝胶体依次经过混捏-冷却成型-石墨化工艺后，加工获得中粗石墨。
优选的，在步骤2中，金属原料包括锌、锆、钛、铝，所述锌、锆、钛、铝质量比为1:1:1:0.5。
优选的，步骤S4中，混捏工艺包括将改性石墨凝胶体用离子水反复清洗数遍，在加入离子水和柠檬酸钠在超声条件下进行搅拌，均匀搅拌后，过滤，过滤后加入油酸作为添加剂进行混捏，混捏时间为30-50min，混捏温度为100-130℃，所述改性石墨凝胶体、柠檬酸钠和油酸的质量比为1:0.2:0.1。
优选的，步骤S4中，冷却成型工艺包括混捏结束后通过挤压机挤压成型，放置一旁静置直至温度降至常温。
优选的，步骤S3中，低温冷冻处理后，将处理后的产物进行超临界二氧化碳发泡处理，发泡结束后，在通过超声处理，处理后，获得改性石墨凝胶体，该改性石墨凝胶体为最终产物。
优选的，S2步骤中，将温度逐渐加热至1100-1200℃时，以流量90-130ml/min向熔炉内通入高纯氩气直至反应结束。
优选的，步骤4中，超声功率为850w，超声频率45-KH。
优选的，步骤3中，超声功率为1000w，超声频率41-KH。
与现有技术相比，本发明的具有以下效果：金属原料可以提高石墨的韧性，锆的耐腐蚀性比钛好、钛重量轻、强度高、具金属光泽，耐湿氯气腐蚀、铝质地坚韧而轻，有延展性，容易导电，还可增强石墨的导电性，将金属原料和石墨搅拌后再通过加入乙醇溶液，使其两者之间融合彻底，在混捏工艺中，加入离子水和柠檬酸钠对石墨凝胶体进行水洗，去除两者混合后产生的杂质，提炼纯度。
具体实施方式
下面结合实施例对发明进行详细的说明。
实施例1
一种高强度的中粗石墨的制备方法，包括以下步骤：
S1、将锻后的石墨焦研磨至干粉状，锻后焦粒含量为60％，焦粒粒度为0.4mm，煅后的焦粉含量为的含量为35％，焦粉的粒度为0.065mm；
S2、选金属原料放入熔炉内，金属原料与石墨焦的质量比为1:12，先预热只100℃，预热时间为10min，预热后，将温度逐渐加热至1100℃，以流量90ml/min向熔炉内通入高纯氩气直至反应结束，加热时间为0.5h，加热后保温30-35min，随后再向熔炉内加入步骤S1获得的石墨焦干粉继续加热30min，随后搅拌，使其均匀充分混合，混合后获得混合物，金属原料包括锌、锆、钛、铝，锌、锆、钛、铝质量比为1:1:1:0.5；
S3、向步骤2中获得的混合物内加入乙醇溶液，该乙醇溶液的浓度为65％。在搅拌速度为1500rpm的条件下搅拌15min使其均匀分散，然后再进行低温冷冻处理，低温冷冻处理后，将处理后的产物进行超临界二氧化碳发泡处理，发泡结束后，在通过超声处理，处理后，获得改性石墨凝胶体，超声功率为1000w，超声频率41-KH；
S4、将改性石墨凝胶体依次经过混捏-冷却成型-石墨化工艺后，加工获得中粗石墨；
混捏工艺包括将改性石墨凝胶体用离子水反复清洗数遍，在加入离子水和柠檬酸钠在超声条件下进行搅拌，均匀搅拌后，过滤，过滤后，加入油酸作为添加剂进行混捏，混捏时间为30min，混捏温度为100℃，改性石墨凝胶体、柠檬酸钠和油酸的质量比为1:0.2:0.1，超声功率为850w，超声频率45-KH；
冷却成型工艺包括混捏结束后通过挤压机挤压成型，放置一旁静置直至温度降至常温。
实施例2
一种高强度的中粗石墨的制备方法，包括以下步骤：
S1、将锻后的石墨焦研磨至干粉状，锻后焦粒含量为62％，焦粒粒度为0.5mm，煅后的焦粉含量为的含量为36％，焦粉的粒度为0.068mm；
S2、选金属原料放入熔炉内，金属原料与石墨焦的质量比为1:12，先预热只135℃，预热时间为11min，预热后，将温度逐渐加热至1150℃，以流量110ml/min向熔炉内通入高纯氩气直至反应结束，加热时间为0.8h，加热后保温32min，随后再向熔炉内加入步骤S1获得的石墨焦干粉继续加热30min，随后搅拌，使其均匀充分混合，混合后获得混合物，金属原料包括锌、锆、钛、铝，锌、锆、钛、铝质量比为1:1:1:0.5；
S3、向步骤2中获得的混合物内加入乙醇溶液，该乙醇溶液的浓度为65％。在搅拌速度为3500rpm的条件下搅拌17min使其均匀分散，然后再进行低温冷冻处理，低温冷冻处理后，将处理后的产物进行超临界二氧化碳发泡处理，发泡结束后，在通过超声处理，处理后，获得改性石墨凝胶体，超声功率为1000w，超声频率41-KH；
S4、将改性石墨凝胶体依次经过混捏-冷却成型-石墨化工艺后，加工获得中粗石墨；
混捏工艺包括将改性石墨凝胶体用离子水反复清洗数遍，在加入离子水和柠檬酸钠在超声条件下进行搅拌，均匀搅拌后，过滤，过滤后，加入油酸作为添加剂进行混捏，混捏时间为35min，混捏温度为120℃，改性石墨凝胶体、柠檬酸钠和油酸的质量比为1:0.2:0.1，超声功率为850w，超声频率45-KH；
冷却成型工艺包括混捏结束后通过挤压机挤压成型，放置一旁静置直至温度降至常温。
实施例3
一种高强度的中粗石墨的制备方法，包括以下步骤：
S1、将锻后的石墨焦研磨至干粉状，锻后焦粒含量为63％，焦粒粒度为0.6mm，煅后的焦粉含量为的含量为38％，焦粉的粒度为0.075mm；
S2、选金属原料放入熔炉内，金属原料与石墨焦的质量比为1:12，先预热只150℃，预热时间为10-15min，预热后，将温度逐渐加热至1200℃，以流量130ml/min向熔炉内通入高纯氩气直至反应结束，加热时间为1.1h，加热后保温30-35min，随后再向熔炉内加入步骤S1获得的石墨焦干粉继续加热30min，随后搅拌，使其均匀充分混合，混合后获得混合物，金属原料包括锌、锆、钛、铝，锌、锆、钛、铝质量比为1:1:1:0.5；
S3、向步骤2中获得的混合物内加入乙醇溶液，该乙醇溶液的浓度为65％。在搅拌速度为4000rpm的条件下搅拌20min使其均匀分散，然后再进行低温冷冻处理，低温冷冻处理后，将处理后的产物进行超临界二氧化碳发泡处理，发泡结束后，在通过超声处理，处理后，获得改性石墨凝胶体，超声功率为1000w，超声频率KH；
S4、将改性石墨凝胶体依次经过混捏-冷却成型-石墨化工艺后，加工获得中粗石墨；
混捏工艺包括将改性石墨凝胶体用离子水反复清洗数遍，在加入离子水和柠檬酸钠在超声条件下进行搅拌，均匀搅拌后，过滤，过滤后，加入油酸作为添加剂进行混捏，混捏时间为50min，混捏温度为130℃，改性石墨凝胶体、柠檬酸钠和油酸的质量比为1:0.2:0.1，超声功率为850w，超声频率45-KH；
冷却成型工艺包括混捏结束后通过挤压机挤压成型，放置一旁静置直至温度降至常温。
对比例1
与实施例2相比，对比例1未以流量90-130ml/min向熔炉内通入高纯氩气直至反应结束，其余同实施例2一致。
对比例2
与实施例2相比，对比例2未加入金属原料，其余同实施例2一致。
对比例3
与实施例2相比，对比例2未在加入离子水和柠檬酸钠在超声条件下进行搅拌，均匀搅拌后，加入油酸作为添加剂进行混捏，其余同实施例2一致。
通过实施例1-3和对比例1-3的制备方法制备出的中粗石墨进行测试，照标准ASTM-D7972和ASTM-D7779，分别测试其弯曲强度和断裂韧性，具体数据见表1；
表1
从表1可知，实施例1-3的弯曲强度和断裂韧性均高于对比例1-3，尤其是实施例2为最优方案。
上述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此理解为对本发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利和保护范围应以所附权利要求书为准。
Claims (7)
1.一种高强度的中粗石墨的制备方法，其特征在于，包括以下步骤：
S1、将锻后的石墨焦研磨至干粉状，锻后焦粒粒度为0.4-0.6mm且焦粒含量为60-63%，煅后的焦粉含量为35-38%，焦粉的粒度为0.065-0.075mm；
S2、选金属原料放入熔炉内，金属原料与石墨焦的质量比为1:12，先预热至100-150℃，预热时间为10-15min，预热后，将温度逐渐加热至1100-1200℃，加热时间为0.5-1.1h，加热后保温30-35min，随后再向熔炉内加入步骤S1获得的石墨焦干粉继续加热30min，随后搅拌，使其均匀充分混合，混合后获得混合物，金属原料包括锌、锆、钛、铝，所述锌、锆、钛、铝质量比为1:1:1:0.5；
S3、向步骤2中获得的混合物内加入乙醇溶液，该乙醇溶液的浓度为65%，在搅拌速度为1500-4000rpm的条件下搅拌15～20min使其均匀分散，然后再进行低温冷冻处理，得到改性石墨凝胶体；
S4、将改性石墨凝胶体依次经过混捏-冷却成型-石墨化工艺后，加工获得中粗石墨。
2.如权利要求1所述的一种高强度的中粗石墨的制备方法，其特征在于，所述步骤S4中，混捏工艺包括将改性石墨凝胶体用去离子水反复清洗数遍，再加入去离子水和柠檬酸钠在超声条件下进行搅拌，均匀搅拌后，过滤，过滤后，加入油酸作为添加剂进行混捏，混捏时间为30-50min，混捏温度为100-130℃，所述改性石墨凝胶体、柠檬酸钠和油酸的质量比为1:0.2:0.1。
3.如权利要求2所述的一种高强度的中粗石墨的制备方法，其特征在于，所述步骤S4中，冷却成型工艺包括混捏结束后通过挤压机挤压成型，放置一旁静置直至温度降至常温。
4.如权利要求1所述的一种高强度的中粗石墨的制备方法，其特征在于，在所述步骤S3中，低温冷冻处理后，将处理后的产物进行超临界二氧化碳发泡处理，发泡结束后，再通过超声处理，处理后，获得改性石墨凝胶体，该改性石墨凝胶体为最终产物。
5.如权利要求1所述的一种高强度的中粗石墨的制备方法，其特征在于，在所述S2步骤中，将温度逐渐加热至1100-1200℃时，以流量90-130mL/min向熔炉内通入高纯氩气直至反应结束。
6.如权利要求3所述的一种高强度的中粗石墨的制备方法，其特征在于，所述步骤S4中，超声功率为850w，超声频率45-KH。
7.如权利要求4所述的一种高强度的中粗石墨的制备方法，其特征在于，所述步骤S3中，超声功率为1000w，超声频率41-KH。
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013001576A (ja) * | 2011-06-10 | 2013-01-07 | Ibiden Co Ltd | 黒鉛材の製造方法および黒鉛材 |
| JP2014181169A (ja) * | 2013-03-21 | 2014-09-29 | Ibiden Co Ltd | 黒鉛材料の製造方法 |
| CN104828809A (zh) * | 2015-04-23 | 2015-08-12 | 成都蓉光炭素股份有限公司 | 一种挤出成型中粗细结构石墨材料的加工方法 |
| CN105624446A (zh) * | 2016-03-22 | 2016-06-01 | 北京工业大学 | 石墨烯增强镁、铝基复合材料及其制备方法 |
| CN107022690A (zh) * | 2017-05-03 | 2017-08-08 | 合肥工业大学 | 一种通过压力浸渗铝合金制备铝/碳基复合材料的方法 |
| CN113564404A (zh) * | 2021-07-13 | 2021-10-29 | 珠海亿特立新材料有限公司 | 一种铝基石墨颗粒增强复合材料及方法和散热转接件 |
| CN113816738A (zh) * | 2021-09-28 | 2021-12-21 | 大同新成新材料股份有限公司 | 一种利用纳米TiO2制备超高导热等静压石墨材料及其方法 |
| CN115466121A (zh) * | 2022-10-28 | 2022-12-13 | 万基控股集团石墨制品有限公司 | 一种石墨电极的制备方法 |
-
2023
- 2023-03-08 CN CN202310216256.5A patent/CN116409993B/zh active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013001576A (ja) * | 2011-06-10 | 2013-01-07 | Ibiden Co Ltd | 黒鉛材の製造方法および黒鉛材 |
| JP2014181169A (ja) * | 2013-03-21 | 2014-09-29 | Ibiden Co Ltd | 黒鉛材料の製造方法 |
| CN104828809A (zh) * | 2015-04-23 | 2015-08-12 | 成都蓉光炭素股份有限公司 | 一种挤出成型中粗细结构石墨材料的加工方法 |
| CN105624446A (zh) * | 2016-03-22 | 2016-06-01 | 北京工业大学 | 石墨烯增强镁、铝基复合材料及其制备方法 |
| CN107022690A (zh) * | 2017-05-03 | 2017-08-08 | 合肥工业大学 | 一种通过压力浸渗铝合金制备铝/碳基复合材料的方法 |
| CN113564404A (zh) * | 2021-07-13 | 2021-10-29 | 珠海亿特立新材料有限公司 | 一种铝基石墨颗粒增强复合材料及方法和散热转接件 |
| CN113816738A (zh) * | 2021-09-28 | 2021-12-21 | 大同新成新材料股份有限公司 | 一种利用纳米TiO2制备超高导热等静压石墨材料及其方法 |
| CN115466121A (zh) * | 2022-10-28 | 2022-12-13 | 万基控股集团石墨制品有限公司 | 一种石墨电极的制备方法 |
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