CN113937273A - 一种电子烟用锂离子电池正极干法匀浆制备工艺 - Google Patents
一种电子烟用锂离子电池正极干法匀浆制备工艺 Download PDFInfo
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 9
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- HFCVPDYCRZVZDF-UHFFFAOYSA-N [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O Chemical compound [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O HFCVPDYCRZVZDF-UHFFFAOYSA-N 0.000 claims description 10
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- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000007580 dry-mixing Methods 0.000 claims description 3
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Abstract
本发明涉及锂电池制备技术领域,具体地说,涉及一种电子烟用锂离子电池正极干法匀浆制备工艺。包括如下步骤:首先将活性物质主材、导电剂和粘接剂干粉混合,放入搅拌缸中常压密封均匀搅拌,然后加入适量溶剂润湿泥状搅拌,高速分散破碎,并稀释调节粘度。本发明设计通过改变投料顺序,改善分散效果,提高浆料的加工性能,使混料均匀、易于涂布,缩短搅拌周期,提高设备利用率,并达到通过改善浆料的分散性、一致性以及粘度细度以提升电池性能的目的,提高电池性能一致性,使电池中值电压显著提高。
Description
技术领域
本发明涉及锂电池制备技术领域,具体地说,涉及一种电子烟用锂离子电池正极干法匀浆制备工艺。
背景技术
锂离子电池制作的关键技术核心在配料工序,材料、配方和匀浆制备工艺的选择将会在很大程度上决定了电池产品的性能。锂电厂的配料普遍选择湿法混料工艺,是将配方所需各项材料逐步加入,并配以搅拌时间和转速,其基本过程为溶胶-导电剂-添加剂-主材,这是目前国内的主流工艺。然而常规配料搅拌的工艺周期长,溶胶、添加导电剂、加上主材的总体搅拌混合时间超过10h,并伴有加工性能不良的忧患,影响涂布效果,分散效果差、涂覆不均匀会导致电池容量分布比较分散。而常规的干法搅拌工艺中,也存在在润湿步骤中,溶剂量、搅拌转速和时间选择不合适导致品质出现问题的情况。然而,目前却没有较为完善的可快速高效完成锂离子电池匀浆浆料的制备工艺。
发明内容
本发明的目的在于提供一种电子烟用锂离子电池正极干法匀浆制备工艺,以解决上述背景技术中提出的问题。
为实现上述技术问题的解决,本发明提供了一种电子烟用锂离子电池正极干法匀浆制备工艺,包括如下步骤:
S1、将粉末状态的锂离子电池正极活性物质镍钴锰酸锂、导电剂SP和粘接剂PVDF按95:2:3的比例称取物料,加入行星搅拌机的搅拌缸中,常压密封均匀搅拌;
S2、进行干混操作,开启公转30rpm、自转800rpm,搅拌时长35min,使各物料干粉充分均匀融合,并开启循环水;
S3、将60%的NMP溶剂加入融合后的干粉中,开启公转35rpm、自转800rpm,搅拌时长40min,再将转速提升至公转45rpm、自转1200rpm,搅拌时长45min,后降下缸体将缸壁内浆料刮落;
S4、将25%的NMP溶剂加入缸内,开启搅拌公转45rpm、自转1200rpm,搅拌时长10min,再将转速提升至公转45rpm、自转1800rpm,搅拌时长20min,再次进行刮料操作;
S5、刮料后加入5%的NMP溶剂,开启搅拌公转45rpm、自转1800rpm,搅拌时长55min,第三次进行刮料操作;
S6、刮料后测试泥状物料的粘度和温度,当泥状物料处于粘度标准4000~7000CPS、温度处于30~40℃内,则开启公转45rpm、自转1800rpm,搅拌时长25min,再次刮料后测试泥状物料的固含量和温度,直到泥状物料处于固含量标准60%~70%、温度处于30~40℃内;
S7、抽真空,使真空度降至-0.07Mpa~-0.095Mpa内,开启公转20rpm、自转0rpm,搅拌时长20min,后关闭循环水,并向搅拌桶内充氮气直到达到1个标准大气压;
S8、出料,控制浆料出料温度为25±3℃。
作为本技术方案的进一步改进,所述S1中,锂离子电池正极活性物质包括但不限于:镍钴锰酸锂(LiNixCoyMn1-x-yO2)、钴酸锂(LiCoO2)、镍酸锂(LiNiO2)、锰酸锂(LiMn2O4)。
作为本技术方案的进一步改进,所述S1中,锂离子电池正极导电剂包括但不限于:导电炭黑(SP)、碳纳米管(CNT)、导电碳黑(350G)、SP-Li、导电石墨(KS6、SFG6)、科琴黑(EC-300J、ECP、ECP-600JD)、VGCF。
作为本技术方案的进一步改进,所述S1中,锂离子电池正极粘接剂包括但不限于:聚偏氟乙烯(PVDF)、偏二氟乙烯(VF2)的均聚物和聚偏二氟乙烯共聚物、偏二氟乙烯(VF2)/六氟丙烯(HFP)的共聚物。
作为本技术方案的进一步改进,所述S1中,锂离子电池正极活性物质采用镍钴锰酸锂,导电剂采用导电炭黑(SP),粘接剂采用聚偏氟乙烯(PVDF)。
作为本技术方案的进一步改进,所述S3中,锂离子电池正极溶剂包括但不限于:N-甲基吡咯烷酮(NMP)。
作为本技术方案的进一步改进,所述S3中,锂离子电池正极溶剂采用固含量为64%的N-甲基吡咯烷酮(NMP)。
作为本技术方案的进一步改进,所述锂离子电池正极浆料配方中的粉末状原料比例为镍钴锰酸锂:SP:PVDF=95:2:3,溶剂采用固含量为64%的NMP。
与现有技术相比,本发明的有益效果:
1.该电子烟用锂离子电池正极干法匀浆制备工艺通过改变传统湿法配料浆料的加工方式,采用干法混料工艺,先将粘结剂、导电剂、主材等物质干粉混合搅拌,随后加入适量的溶剂润湿泥状物料并进行高速分散破碎,最后加入溶剂进行稀释调节粘度,以适合涂布;
2.该电子烟用锂离子电池正极干法匀浆制备工艺通过改变投料顺序,改善分散效果,提高浆料的加工性能,使混料均匀、易于涂布,缩短搅拌周期,提高设备利用率,并达到通过改善浆料的分散性、一致性以及粘度细度以提升电池性能的目的,提高电池性能一致性,使电池中值电压显著提高。
附图说明
图1为本发明的整体制备工艺流程框图;
图2为本发明的整体工艺方法流程图。
具体实施方式
下面将结合本发明实施例中的附图,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做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
如图1-图2所示,本实施例的目的之一在于,提供了一种电子烟用锂离子电池正极干法匀浆制备工艺,包括如下步骤:
S1、将粉末状态的锂离子电池正极活性物质镍钴锰酸锂、导电剂SP和粘接剂PVDF按95:2:3的比例称取物料,加入行星搅拌机的搅拌缸中,常压密封均匀搅拌;
S2、进行干混操作,开启公转30rpm、自转800rpm,搅拌时长35min,使各物料干粉充分均匀融合,并开启循环水;
S3、将60%的NMP溶剂加入融合后的干粉中,开启公转35rpm、自转800rpm,搅拌时长40min,再将转速提升至公转45rpm、自转1200rpm,搅拌时长45min,后降下缸体将缸壁内浆料刮落;
S4、将25%的NMP溶剂加入缸内,开启搅拌公转45rpm、自转1200rpm,搅拌时长10min,再将转速提升至公转45rpm、自转1800rpm,搅拌时长20min,再次进行刮料操作;
S5、刮料后加入5%的NMP溶剂,开启搅拌公转45rpm、自转1800rpm,搅拌时长55min,第三次进行刮料操作;
S6、刮料后测试泥状物料的粘度和温度,当泥状物料处于粘度标准4000~7000CPS、温度处于30~40℃内,则开启公转45rpm、自转1800rpm,搅拌时长25min,再次刮料后测试泥状物料的固含量和温度,直到泥状物料处于固含量标准60%~70%、温度处于30~40℃内;
S7、抽真空,使真空度降至-0.07Mpa~-0.095Mpa内,开启公转20rpm、自转0rpm,搅拌时长20min,后关闭循环水,并向搅拌桶内充氮气直到达到1个标准大气压;
S8、出料,控制浆料出料温度为25±3℃。
本实施例中,所述S1中,锂离子电池正极活性物质包括但不限于:镍钴锰酸锂(LiNixCoyMn1-x-yO2)、钴酸锂(LiCoO2)、镍酸锂(LiNiO2)、锰酸锂(LiMn2O4)。
进一步地,所述S1中,锂离子电池正极导电剂包括但不限于:导电炭黑(SP)、碳纳米管(CNT)、导电碳黑(350G)、SP-Li、导电石墨(KS6、SFG6)、科琴黑(EC-300J、ECP、ECP-600JD)、VGCF。
进一步地,所述S1中,锂离子电池正极粘接剂包括但不限于:聚偏氟乙烯(PVDF)、偏二氟乙烯(VF2)的均聚物和聚偏二氟乙烯共聚物、偏二氟乙烯(VF2)/六氟丙烯(HFP)的共聚物。
具体地,所述S1中,锂离子电池正极活性物质采用镍钴锰酸锂,导电剂采用导电炭黑(SP),粘接剂采用聚偏氟乙烯(PVDF)。
本实施例中,所述S3中,锂离子电池正极溶剂包括但不限于:N-甲基吡咯烷酮(NMP)。
具体地,锂离子电池正极溶剂采用固含量为64%的N-甲基吡咯烷酮(NMP)。
本实施例中,所述锂离子电池正极浆料配方中的粉末状原料比例为镍钴锰酸锂:SP:PVDF=95:2:3,溶剂采用固含量为64%的NMP。
进一步地,S3、S4、S5中添加的溶剂,均可通过对固含量为64%的NMP进行稀释配制得到。
具体地,每次添加溶剂时,可根据粉末状原料的量或泥状原料的量按需缓慢添加,其中:第一次添加溶剂的作用是润湿粉末物料,使粉末物料可以粘接成团;第二次添加溶剂的作用是润湿泥状物料,便于分散破碎物料;第三次添加溶剂的作用是调节粘度,使成品浆料的浆质更均匀。
此外,添加溶剂的次数可根据物料的量及状态进行调整。
另外,本实施例还提供了一种通过上述的电子烟用锂离子电池正极干法匀浆制备工艺制备匀浆浆料的实验操作,其具体步骤如下:
Step1、首先将300kg镍钴锰酸锂、6.31kg导电炭黑(Super-P)和9.47g聚偏氟乙烯(PVDF)放入搅拌缸中常压密封均匀搅拌,搅拌缸公转速度为25rpm,搅拌缸自转速度为200rpm,搅拌时间30min;
Step2、然后加入65.06kgCNT(碳纳米管),低速搅拌公转速度为5rpm,搅拌缸自转速度为0rpm,搅拌时间5min;
Step3、开启冷却水,完成搅拌后,将公转速度调整为25rpm,搅拌缸自转速度为0rpm,搅拌时间60min;
Step4、然后测试浆料温度为29℃,加入适量溶剂NMP(N-甲基吡咯烷酮)润湿泥状搅拌,将公转速度调整为20rpm,搅拌缸自转速度为1500rpm,搅拌时间15min,高速分散破碎;
Step5、第二次加入适量溶剂NMP(N-甲基吡咯烷酮)调节粘度,真空搅拌,将公转速度调整为25rpm,搅拌缸自转速度为1800rpm,搅拌时间55min;
Step6、待浆料温度降至45℃以下,然后得到均匀稳定的镍钴锰酸锂锂离子电池正极干法匀浆浆料。
本发明的电子烟用锂离子电池正极干法匀浆制备工艺通过改变传统湿法配料浆料的加工方式,采用干法混料工艺,先将粘结剂、导电剂、主材等物质干粉混合搅拌,随后加入适量的溶剂润湿泥状物料并进行高速分散破碎,最后加入溶剂进行稀释调节粘度,以适合涂布;
本发明的电子烟用锂离子电池正极干法匀浆制备工艺通过改变投料顺序,改善分散效果,提高浆料的加工性能,使混料均匀、易于涂布,缩短搅拌周期,提高设备利用率,并达到通过改善浆料的分散性、一致性以及粘度细度以提升电池性能的目的,提高电池性能一致性,使电池中值电压显著提高。
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仅为本发明的优选例,并不用来限制本发明,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。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (8)
1.一种电子烟用锂离子电池正极干法匀浆制备工艺,其特征在于:包括如下步骤:
S1、将粉末状态的锂离子电池正极活性物质镍钴锰酸锂、导电剂SP和粘接剂PVDF按95:2:3的比例称取物料,加入行星搅拌机的搅拌缸中,常压密封均匀搅拌;
S2、进行干混操作,开启公转30rpm、自转800rpm,搅拌时长35min,使各物料干粉充分均匀融合,并开启循环水;
S3、将60%的NMP溶剂加入融合后的干粉中,开启公转35rpm、自转800rpm,搅拌时长40min,再将转速提升至公转45rpm、自转1200rpm,搅拌时长45min,后降下缸体将缸壁内浆料刮落;
S4、将25%的NMP溶剂加入缸内,开启搅拌公转45rpm、自转1200rpm,搅拌时长10min,再将转速提升至公转45rpm、自转1800rpm,搅拌时长20min,再次进行刮料操作;
S5、刮料后加入5%的NMP溶剂,开启搅拌公转45rpm、自转1800rpm,搅拌时长55min,第三次进行刮料操作;
S6、刮料后测试泥状物料的粘度和温度,当泥状物料处于粘度标准4000~7000CPS、温度处于30~40℃内,则开启公转45rpm、自转1800rpm,搅拌时长25min,再次刮料后测试泥状物料的固含量和温度,直到泥状物料处于固含量标准60%~70%、温度处于30~40℃内;
S7、抽真空,使真空度降至-0.07Mpa~-0.095Mpa内,开启公转20rpm、自转0rpm,搅拌时长20min,后关闭循环水,并向搅拌桶内充氮气直到达到1个标准大气压;
S8、出料,控制浆料出料温度为25±3℃。
2.根据权利要求1所述的电子烟用锂离子电池正极干法匀浆制备工艺,其特征在于:所述S1中,锂离子电池正极活性物质包括但不限于:镍钴锰酸锂(LiNixCoyMn1-x-yO2)、钴酸锂(LiCoO2)、镍酸锂(LiNiO2)、锰酸锂(LiMn2O4)。
3.根据权利要求2所述的电子烟用锂离子电池正极干法匀浆制备工艺,其特征在于:所述S1中,锂离子电池正极导电剂包括但不限于:导电炭黑(SP)、碳纳米管(CNT)、导电碳黑(350G)、SP-Li、导电石墨(KS6、SFG6)、科琴黑(EC-300J、ECP、ECP-600JD)、VGCF。
4.根据权利要求3所述的电子烟用锂离子电池正极干法匀浆制备工艺,其特征在于:所述S1中,锂离子电池正极粘接剂包括但不限于:聚偏氟乙烯(PVDF)、偏二氟乙烯(VF2)的均聚物和聚偏二氟乙烯共聚物、偏二氟乙烯(VF2)/六氟丙烯(HFP)的共聚物。
5.根据权利要求4所述的电子烟用锂离子电池正极干法匀浆制备工艺,其特征在于:所述S1中,锂离子电池正极活性物质采用镍钴锰酸锂,导电剂采用导电炭黑(SP),粘接剂采用聚偏氟乙烯(PVDF)。
6.根据权利要求1所述的电子烟用锂离子电池正极干法匀浆制备工艺,其特征在于:所述S3中,锂离子电池正极溶剂包括但不限于:N-甲基吡咯烷酮(NMP)。
7.根据权利要求6所述的电子烟用锂离子电池正极干法匀浆制备工艺,其特征在于:所述S3中,锂离子电池正极溶剂采用固含量为64%的N-甲基吡咯烷酮(NMP)。
8.根据权利要求7所述的电子烟用锂离子电池正极干法匀浆制备工艺,其特征在于:所述锂离子电池正极浆料配方中的粉末状原料比例为镍钴锰酸锂:SP:PVDF=95:2:3,溶剂采用固含量为64%的NMP。
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