CN112105452A - 流化床反应器 - Google Patents
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Abstract
根据本发明的用于制造碳纳米管的流化床反应器包括:反应器主体,其在纵向上具有中空的形状;分散板,其具有板状,并且安装在所述反应器主体内以在横向上分隔反应器主体的内部,并且在所述分散板中形成有多个供反应气体通过的穿孔;喷嘴单元,其安装在分散板的一个表面上,以接收来自外部的惰性气体并注入惰性气体,从而粉碎沉积在分散板上的沉积物;感测单元,其被配置为感测沉积在分散板上的沉积物的沉积状态;以及控制单元,其被配置为根据在所述感测单元中感测到的信息来控制喷嘴单元的操作。根据具有如上所述的技术特征的本发明,可以通过感测单元感测反应器主体内的沉积物,并且可以通过喷嘴单元将其粉碎,以进一步提高碳纳米管的生产效率。
Description
相关申请的交叉引用
本申请要求于2019年2月28日提交的韩国专利申请第10-2019-0024231号的优先权的权益,其全部内容通过引用并入本文。
技术领域
本发明涉及一种用于制造碳纳米管的流化床反应器,更具体地,本发明涉及一种流化床反应器,其中设置感测单元以掌握在分散板上沉积的沉积物的状态,以及在分散板上设置喷嘴单元以通过注入惰性气体来粉碎所述沉积物。
背景技术
碳纳米管(CNT)是其中彼此相邻的三个碳原子以六边形蜂窝结构彼此键合成碳平面,且碳平面以圆柱形状卷曲以形成管的材料。碳纳米管作为在各种技术领域中广泛应用的新材料而备受关注。例如,将碳纳米管应用于诸如电磁屏蔽装置的电化学存储装置的电极,显示装置,或气体传感器以及二次电池,全电池等。
作为制造碳纳米管的方法,已经公开了电弧放电法、激光蒸发法、化学气相沉积法等。
在它们中,在化学气相生长方法中,通常,金属催化剂颗粒和基于烃的反应气体在高温流化床反应器中彼此反应以产生碳纳米管。
参见图1,根据现有技术的流化床反应器的示意性构造,左图示出了反应器主体1的外观,右图(当以一定距离从上侧向下观察时)示出了由反应器主体1的内部观察,安装了分散板2的状态,流化床反应器包括在纵向方向上具有中空的圆柱形管形状的反应器主体1,并且具有如下的结构:反应器主体1的入口1a具有锥形形状,并且注入到入口1a中的反应气体通过在分散板2中打穿的穿孔2a而排放到出口1b。
反应器主体1可以选择性地连接至加热器(未示出),以便在高温下加热。在反应气体流动的同时,用反应器主体1合成了在反应器主体1中提供的催化剂金属以制造CNT。
这里,分散板2将反应气体均匀地分散在反应器主体1内,并使反应气体通过,从而防止反应产生的催化剂金属和粉末掉落。
即,在流化床反应器中,当金属催化剂被放置在分散板2上,从下侧通过穿孔2a向上供应反应气体时,金属催化剂在反应的同时在分散板2上方流动。
然而,如图1b所示,其示出了在CNT的合成过程中反应器主体1的内部,在CNT的合成过程中,由催化剂金属颗粒生长的次级颗粒彼此集聚形成块,然后产生沉积物,随着时间的流逝沉积物变得越来越硬。
沉积物的产生在反应器主体1中引起各种问题。例如,在图1b中形成沉积物的区域中,沉积物堵住分散板2的穿孔2a,从而中断了反应气体的流动,由此不利地影响了CNT的合成。沉积物在反应器主体1中彼此集聚,从而导致缺陷以及各种传感器和装置的故障。
为了解决这些问题,根据现有技术,在反应器主体1的内部或外部安装振动器以施加振动,或者采用在反应器主体1内旋转的叶轮将沉积物粉碎。
然而,CNT的合成在600度至1,000度的高温下进行。另外,由于使用诸如乙烯、甲烷等的易燃气体作为反应气体,所以由于振动器的振动和叶轮的旋转而引起的物理冲击是引起火灾危险的危险因素。而且,在根据现有技术的方法中,难以完全粉碎沉积物。
发明内容
技术问题
因此,本发明的主要目的是提供一种流化床反应器,其能够检测在分散板上生成的沉积物的产生并且能够有效地粉碎和去除所产生的沉积物。
技术方案
为了实现上述目的,根据本发明的用于制造碳纳米管的流化床反应器包括:反应器主体,其在纵向上具有中空的形状;分散板,其具有板状,并且安装在所述反应器主体内以在横向上分隔反应器主体的内部,并且在所述分散板中形成有多个供反应气体通过的穿孔;喷嘴单元,其安装在所述分散板的一个表面上,以接收来自外部的惰性气体并注入惰性气体,从而粉碎沉积在分散板上的沉积物;感测单元,其被配置为感测沉积在分散板上的沉积物的沉积状态;以及控制单元,其被配置为根据在所述感测单元中感测到的信息来控制喷嘴单元的操作。
所述分散板可以具有板状,并且可以设置多个喷嘴单元,所述喷嘴单元被设置成沿着分散板的周边彼此间隔开。
根据本发明的喷嘴单元可以包括:壳体,其固定至分散板的一个表面上,沉积物在该表面上堆积;供应管线,其被配置为将来自外部的惰性气体供应到壳体中;和注入部,其设置在壳体中以注入惰性气体。
可以在所述壳体中设置两个或更多个注入部,以沿不同方向注入惰性气体。另外,可以将在壳体中设置的至少一个注入部设置为向其相邻的壳体注入惰性气体。
所述感测单元可以包括温度计,该温度计被设置为与分散板的沉积物在其上堆积的一个表面相隔预定距离,并且所述控制单元可以根据温度变化来估计沉积物的堆积量。
可以设置多个温度计,它们被设置为沿着分散板的周边彼此间隔。优选地,可以设置多个温度计,它们被设置在距分散板的不同距离处。
温度计可以是配置为通过直接接触沉积物来测量温度的接触式温度计,或者可以是被设置在不接触沉积物的位置以通过感测从沉积物发出的光能来测量温度的非接触式温度计。但是,由于反应器主体的内部温度较高,因此,根据发生故障的可能性、测量可靠性和耐久性,优选使用接触式温度计。
有益效果
根据具有上述技术特征的本发明,可通过感测单元感测反应器主体内的沉积物,并通过喷嘴单元将其粉碎以进一步提高碳纳米管的生产效率。
由于多个喷嘴单元沿分散板的周边彼此间隔地设置,因此可以使惰性气体未及的遮蔽部分最小化或抑制这样的遮蔽部分,以更有效地粉碎沉积物。
另外,所述喷嘴单元可以在每个壳体中设置有两个或更多个注入部,以沿更多个不同方向注入惰性气体。
此外,可以安装多个构成感测单元的温度计,以便根据每个点的温度差有效地感测沉积物的产生状态。
附图说明
图1a是示出根据现有技术的流化床反应器的构造的示意图,其中,左图示出了反应器主体的外观,右图示出了由反应器的内部观察安装了分散板的状态。
图1b是示出在CNT合成期间图1a的反应器主体内部的剖视图。
图2是示出根据本发明实施方式的流化床反应器的内部构造的示意图,其中左图示出了反应器主体的外观,右图示出了由反应器的内部观察,安装了包括温度计和喷嘴单元的分散板的状态。
图3a是由喷嘴单元观察,安装了喷嘴单元的分散板部分的放大图。
图3b是具有不同变形形状的喷嘴单元的透视图。
图4a是示出根据本发明的实施方式1在反应器主体的四个点处以相同高度设置温度计的状态的视图(左:从上侧至下侧的透视图,右:从外部的主视图)。
图4b是示出根据本发明的实施方式2在反应器主体的三个点处以彼此不同的高度设置温度计的状态的视图(左:从上侧至下侧的透视图,右:从外部的主视图)。
图4c是根据本发明的实施方式3在反应器主体内部在彼此不同的高度处安装温度计(每个温度计具有环形形状)的状态的透视图。
图5是示出根据现有技术在流化床反应器中沉积物堆积的状态a以及根据本发明在流化床反应器中沉积物被粉碎的状态b的示意图。
具体实施方式
在下文中,将参照附图详细描述本发明的优选实施方式,使得本发明所属领域的技术人员可以容易地实施本发明的技术思想。然而,本发明可以以不同的形式实施,并且不应被解释为限于这里阐述的实施方式。
为了清楚地说明本发明,省略了与说明书无关的部分,并且在整个说明书中,相同或相似的部件由相同的附图标记表示。
另外,在本说明书和权利要求书中使用的术语或词语不应被限制性地解释为普通含义或基于字典的含义,而应基于发明人可以适当地定义术语的概念,以便以最佳方式描述和解释他或她的发明的原则而解释为符合本发明范围的含义和概念。
本发明涉及用于制造碳纳米管的流化床反应器。在下文中,将参考附图更详细地描述本发明。
参考图2,其示出了根据本发明实施方式的流化床反应器的内部构造,其中左图示出了反应器主体的外观,右图示出了通过由反应器主体观察其中安装了包括温度计及喷嘴单元的分散板的状态,参考图3a和图3b,其示出了根据本发明的具有如下结构的流化床反应器,其中,具有圆形板状的分散板20安装在纵向上具有中空的圆柱形管形状的反应器主体10中。
安装分散板20以在横向上分隔反应器主体10的内部,并且多个穿孔21均匀地分布在分散板20中,使得从反应器主体10的入口10a流向出口10b的反应气体通过。
此外,喷嘴单元和感测单元安装在其上合成碳纳米管的表面(形成沉积物的表面)上,并且喷嘴单元30和感测单元电连接或无线连接至控制单元以便与控制单元进行通讯。控制单元连接到包括供应装置的外部装置,该供应装置将惰性气体供应到喷嘴单元30,以便基于由感测单元提供的信息来控制喷嘴单元30的操作。控制单元可以与控制流化床反应器的软件或硬件组合,或者可以以单独的设备另外设置控制单元。
喷嘴单元30被构造成接收从外部供应的惰性气体(例如,氮气)并在适当的压力条件下将惰性气体喷射到沉积在分散板20上的沉积物上,从而粉碎沉积物。
喷嘴单元30(30a和30b)包括固定在分散板20的一个沉积物在其上堆积的表面上的壳体31。壳体31可以具有如图3a和3b所示的圆柱形或棱柱形形状,在不对催化金属和反应气体的流动和合成造成干扰的范围内,对其尺寸和形状没有限制,其可以设置为固定在分散板20上。作为参考,当气体和催化剂金属流动时,与图3a所示的棱柱形壳体31相比,图3b所示的圆柱形的壳体31可以产生较小的流动阻力。壳体31的尺寸和形状可以根据以下描述的温度计40的布置结构和反应器主体10的内部设计确定为各种形式,如多面体形状、圆柱形状和圆锥形状。
壳体31连接到反应器主体10的外部,使得从外部惰性气体存储装置(未示出)供应惰性气体的供应管线32的一端连接到其上。供应管线32可将以适当压力从外部存储装置供应的惰性气体供应到壳体31。如图2所示,一条供应管线32可以连接到一个壳体31,或者一条供应管线32可以连接到多个壳体31。
由于在供应管线32的末端在壳体31内注入惰性气体的截面积减小,在壳体31上安装或形成注入部33,使得在注入惰性气体的同时,压力能量转换为速度能量。注入部33具有惰性气体流过的流路面积小于供应管线32的流路面积的结构,因此以足够的压力和速度注入惰性气体,在该压力和速度下,沉积物能够被粉碎。
如图3a和3b所示,尽管在本发明中在一个壳体31中设置一个注入部33,但是优选地,在一个壳体31中设置两个注入部33以沿不同方向注入惰性气体(这里,可以设置超过两个注入部的多个注入部以在多个方向上注入惰性气体。在这种情况下,在供应惰性气体时必须施加足够高的压力)。
另外,如图2所示,在圆形分散板20的边缘附近沿周边以规则的间隔规则地布置有多个喷嘴单元30。此外,设置至少一个布置在壳体31中的注入部33以将惰性气体沿着分散板20的周边向相邻的壳体31注入。如图5所示,其示出了其中沉积物在根据现有技术的流化床反应器中堆积的简化的状态(a),以及其中沉积物在根据本发明的流化床反应器中被粉碎的简化的状态(b),这样做是为了更有效地粉碎在分散板20和反应器主体10彼此接触的边缘部分上更易于堆积的沉积物。
此外,感测在分散板20上沉积的沉积物的沉积状态的感测单元被设置为温度计40。
温度计40可以是用于通过感测从沉积物发出的光能来测量温度的非接触式温度计。然而,在非接触式温度计的情况下,由于反应器主体10的内部具有600度以上的高温,因此考虑到故障的可能性和可靠性,优选使用通过直接接触沉积物来测量温度的接触式温度计。
多个温度计40(像喷嘴单元一样)可以被设置为沿着分散板20的周边彼此间隔开,以将温度信息传输到控制单元。控制单元可以根据在反应过程中在温度计40中测量的温度偏差来预测和检测沉积物的产生。
即,当在特定部分产生沉积物时,反应气体可能不能通过该特定部分,因此,合成可能无法适当地进行。结果,最靠近该特定部分的温度计可以测量到比其他温度计更低的温度,由此,控制单元可以估计沉积物产生的位置和量以控制喷嘴单元30的操作,从而粉碎沉积物。
此外,根据本发明的温度计40具有棒或环形形状,并且温度计40的一部分位于反应器主体10内部以实时测量内部温度,温度计40的一部分位于反应器主体10的外部以便将数据传输到控制单元/从控制单元接收数据。
根据温度计40的布置,本发明提供了三个实施方式。
参照图4a,其示出了根据本发明的实施方式1将温度计设置在反应器主体10中具有相同高度的四个位置处的状态(左:由反应器主体观察,从上侧向下观看的透视图,右:从外部观看的主视图)(作为参考,图4a至图4c仅示出了温度计,而未示出喷嘴单元,以防止附图中的线彼此重叠),根据实施方式1的温度计40具有相同形状并且设置在反应器主体10中相同高度处。
这里,温度计40具有棒状形状,并且可以被配置为通过一个温度计40测量各个点的温度。例如,独立地测量三个点(这三个点分为:离反应器主体10的内周边面相对较近的点,离反应器主体10的内周面相对较远的点,以及在该较近点与较远点之间的点)处的温度的温度传感器分别被设置成各自通过一个温度计40测量这三个点处的温度。因此,如图4a所示,如果安装四个温度计40,则可以在十二个点处分别测量温度。当然,如果将更多的温度传感器连接到每个温度计40,则可以在更多的点处进行更详细的温度测量。
另外,参照图4b,其示出根据本发明的实施方式2将三个温度计40设置在反应器主体中不同高度的状态(左:从上侧观察的透视图,右:从外部观察的主视图),根据实施方式2,温度计具有相同的形状,并且设置在反应器主体10内不同的高度处。
在该实施方式中,温度计40具有棒状的形状,并且可以被配置为通过一个温度计40来测量各个点处的温度。此外,温度计可以被设置在不同的高度处以测量沉积物的高度(量)。即,如果由设置在相对较高位置的点A处设置的温度计测量的温度是正常的,而由设置在点C和点B处的温度计测量的温度异常,则可以根据异常程度估计沉积物的高度。
参照图4c,其示出了根据本发明的实施方式3将环形温度计40安装在反应器主体10中不同高度处的状态,在环形温度计40中,可以将多个温度传感器径向地设置以便更有效地感测沉积物的堆积位置和高度。然而,由于在合成碳纳米管时可能干扰催化剂金属和反应气体的流动,因此碳纳米管的尺寸和形状可能受到限制。
在根据本发明的具有上述技术特征的流化床反应器中,可以通过感测单元感测反应器主体10内的沉积物,并且可以通过喷嘴单元30有效地粉碎沉积物以进一步提高碳纳米管的生产效率。
Claims (10)
1.用于制造碳纳米管的流化床反应器,其包括:
反应器主体,其在纵向上具有中空的形状;
分散板,其具有板状,并且安装在所述反应器主体内以在横向上分隔所述反应器主体的内部,并且在所述分散板中形成有多个供反应气体通过的穿孔;
喷嘴单元,其安装在所述分散板的一个表面上,以接收来自外部的惰性气体并注入所述惰性气体,从而粉碎沉积在所述分散板上的沉积物;
感测单元,其被配置为感测沉积在所述分散板上的沉积物的沉积状态;以及
控制单元,其被配置为根据在所述感测单元中感测到的信息来控制所述喷嘴单元的操作。
2.根据权利要求1所述的流化床反应器,其中,所述分散板具有板状,并且所述喷嘴单元设置为多个,并被设置为沿所述分散板的周边彼此间隔开。
3.根据权利要求2所述的流化床反应器,其中,所述喷嘴单元包括:
壳体,其被固定至所述分散板一个表面,所述沉积物在该表面上堆积;
供应管线,其被配置为将来自外部的惰性气体供应到所述壳体中;以及
注入部,其设置在所述壳体中以注入所述惰性气体。
4.根据权利要求3所述的流化床反应器,其中,在所述壳体中设置有两个或更多个注入部,以沿不同方向注入所述惰性气体。
5.根据权利要求4所述的流化床反应器,其中,设置在所述壳体中的至少一个注入部被设置为向与其相邻的壳体注入所述惰性气体。
6.根据权利要求1至5中任一项所述的流化床反应器,其中,所述感测单元包括温度计,其被设置为与所述分散板的一个沉积物在其上堆积的表面相隔预定距离,并且
所述控制单元根据温度变化估计沉积物的堆积量。
7.根据权利要求6所述的流化床反应器,其中,所述温度计设置为多个,它们被设置为沿着所述分散板的周边彼此间隔开。
8.根据权利要求6所述的流化床反应器,其中,所述温度计设置为多个,它们被设置在距所述分散板的不同距离处。
9.根据权利要求6所述的流化床反应器,其中,所述温度计是被配置为通过直接接触所述沉积物来测量温度的接触式温度计。
10.根据权利要求6所述的流化床反应器,其中,所述温度计是被设置在不接触所述沉积物的位置以通过感测从所述沉积物发出的光能来测量温度的非接触式温度计。
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- 2020-01-20 WO PCT/KR2020/000929 patent/WO2020175800A1/ko unknown
- 2020-01-20 US US17/053,944 patent/US11173463B2/en active Active
- 2020-01-20 CN CN202080002716.9A patent/CN112105452B/zh active Active
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TW202045249A (zh) | 2020-12-16 |
TWI807169B (zh) | 2023-07-01 |
US20210220790A1 (en) | 2021-07-22 |
KR102422089B1 (ko) | 2022-07-18 |
KR20200105270A (ko) | 2020-09-07 |
CN112105452B (zh) | 2022-12-23 |
JP7216810B2 (ja) | 2023-02-01 |
JP2021523006A (ja) | 2021-09-02 |
EP3778003A1 (en) | 2021-02-17 |
WO2020175800A1 (ko) | 2020-09-03 |
US11173463B2 (en) | 2021-11-16 |
EP3778003A4 (en) | 2021-05-05 |
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