CN1458966A - 将含碳原料转变为有清晰纳米结构含碳材料的装置和方法 - Google Patents

将含碳原料转变为有清晰纳米结构含碳材料的装置和方法 Download PDF

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CN1458966A
CN1458966A CN01815791A CN01815791A CN1458966A CN 1458966 A CN1458966 A CN 1458966A CN 01815791 A CN01815791 A CN 01815791A CN 01815791 A CN01815791 A CN 01815791A CN 1458966 A CN1458966 A CN 1458966A
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plasma gas
gas
raw material
carbon
carbon black
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F·法布里
E·格里维
N·普罗布斯特
R·斯梅特
J－Y佩罗埃
G·福拉蒙特
L·法彻里
P·雷洛克斯
F·菲舍尔
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Imerys Graphite and Carbon Switzerland SA
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Abstract

公开了通过转变含碳原料制造炭黑或含碳化合物的装置和方法，该方法包括以下步骤：用电能产生等离子体气体，引导所述等离子体气体经过文丘里管，该管的直径沿等离子体气体流动方向变窄，将所述等离子体气体导入反应区，在反应区占优势的空气动力和电磁力产生的流动条件下，原料没有明显的再循环，在反应区中将原料注入等离子体气体，从反应区回收反应产物，将炭黑或含碳化合物与其它反应产物分离。

Description

将含碳原料转变为有清晰纳米结构含碳材料的装置和方法
本发明涉及将含碳原料转变为炭黑或其它含碳材料、尤其是具有清晰(defined)纳米结构含碳材料的方法和装置。
目前，超过99％的炭黑通过不完全燃烧方法制得，迄今为止最主要的方法是六十年前发展起来的“炉法”，其它方法有“通道法”、“热法”和“灯法”。所有这些工业方法的特征是有大约40-60％的原料或原材料的燃烧产生裂解剩余原料所需的热量。即便生产厂家目前提供了超过100种等级的炭黑，每种等级具有不同的供特定用途的规格和性能，但是新材料的生产仍受到工艺化学(化学组成、可获得的能量方面)的限制。
全球每年生产大约6百万MT(公吨)的炭黑。用作原料的原材料是用于低质量材料(轮胎生产)的滗析油(decant oil)、裂解燃料油(pyrolysis fuel oil，PFO)和煤焦油馏出物。一千两百万公吨用来制造炭黑的油所得的污染物排放为两千两百万公吨CO2和数百万公吨的SOx和NOx。进行乙炔的自分解来生产高等级炭黑(40 000 MT)，主要用于电池制造。
还开发了另一种工业规模上基于电等离子体为主要能源的技术，该技术以直流(DC)碳电极等离子体发生器为基础。PCT/NO92/00196和PCT/NO96/00167揭示这样的等离子体反应器。根据所揭示的内容，主要产物是氢，次要产物是碳材料。但是，无证据表明该方法能够生产有商业价值的炭黑。
PCT/EP94/00321揭示了具有三个电极的等离子体反应器，通过向电极施加交流电来产生复合弧。将原料经过弧区加入反应器中。根据该现有技术，反应区位于弧区的正下方且与其相邻，在该反应区中原料转变为具有清晰纳米结构的碳化合物(即转变为炭黑)。原料至少是部分循环经过弧区。该方法制得的炭黑是由多种热处理得到的碳材料的混合物。该方法使得能制备不同的炭黑材料。
因此，本发明的目的是提供一种制备具有完好性能的炭黑的方法和装置，使得通过控制操作条件和工艺参数而获得原料的高转化效率和可再现的产品质量。
本发明通过权利要求书中限定的方法和装置来实现该发明目的。另外，一种新炭黑是本发明的另一个实施方案。本发明的较佳实施方案由从属权利要求限定。下文和具体实施例以及附图将说明本发明的特征，这些特征的组合或次组合构成另一些实施方案。
本发明可以控制操作条件来制造具有明确性能的炭黑，并防止原料和任何产物循环经过弧区，由此制得具有明确且可恒定再现的性能的炭黑材料。特别是文丘里管使得能更好地控制反应温度，并在“低温区域”即制备炭黑的反应区内获得更有效的混合物。
本发明的一大优点是可以使用几乎所有的含碳原料。更具体而言，燃烧焓低(例如低于80 BMCI)的材料，包括轮胎热解得到的再循环油也可用作原料。
较佳的方法包括以下步骤：使等离子体气体经过电弧产生等离子体，让等离子体气体经过或引导等离子体气体经过文丘里管区(该区的直径在等离子体气体流动方向的喉部变窄)，将等离子体气体通入或导入反应区(该区的直径大于文丘里管区的喉部)，(在等离子体气体经过文丘里管区喉部之后)将原料注入位于在文丘里管区后面的反应区内的等离子体气体中，从反应区中提取反应产物并回收炭黑。也可以将原料注入文丘里管的喉部和/或文丘里管稍上方的位置。
与其它反应产物分离的炭黑具有清晰的纳米结构。该纳米结构的形态和织构取决于操作条件。
将等离子体气体注入反应区空间中，不一定要通过等离子体弧。在一个较佳实例中，电弧是一种由至少三个电极产生的复合弧。优选是，电极是以石墨为基的电极，电弧是将电极接到足够的交流电源上而产生的。电流频率可以是使用常规电源(50-60Hz)的栅极(grid)的频率，也可以通过使用高频功率切换电源而更高。升高频率适合于提高电弧稳定性，尤其是当使用氢气作为等离子体气体时。这时，电流频率优选是在500Hz至10kHz之间。
文丘里管较好是由石墨基材料制得，成形为锥形。文丘里管的出口段优选是成形为陡的边缘(edge)，从而形成一个突然扩张的区域。喉部和该突然扩张的区域之间的边缘导致等离子体气体体积急剧膨胀。这一手段较好地防止了含碳材料回流到文丘里管区入口前面的区域，尤其是防止含碳材料回流到等离子体形成区(如弧区)中。同时，扩张区还在物流中产生一高湍流区，用来提高等离子体流和原料之间的混合效率，从而实现均匀混合且更好地控制反应温度。
原料可以含有甲烷、乙炔、乙烯、丙烯、C4-烃(包括丁二烯)、轻油或重油、甚至是废油和/或裂解燃料油(PFO)，以及任何其它含碳材料，或者原料可以是由上述材料组成。优选是，基本上不将氧气或含氧材料加入弧中和反应器中。可以使用分子中含有限量氧的原料，例如氧/碳的原子比最多为1/6。
较好是，等离子体气体在电极上方轴向注入，为的是使等离子体气体直接经过弧。等离子体气体本身可以优选包含下列气体或者由这些气体组成：氢气、氮气、一氧化碳、氩气、氦气或其它合适气体，以及上述气体的混合物，例如最多50％(体积)CO和氢气的混合气。尾气中所含的除等离子体气体以外的其它组分主要只是氢、甲烷、乙炔和乙烯，因此相对独立于烃原料。若使用氧化合物，则尾气中含有一些CO和非常少量的CO2。
优选是一部分尾气再循环用作等离子体气体。若再循环的尾气主要只由氢气和痕量烃组成，那就特别好。
优选是通过调节等离子体气体的流量、电能和原料流量来将反应区中的温度控制在900℃至3000℃的范围内。
用至少一个注射器，优选是用两个至五个注射器注入原料。这些注射器可以环绕反应区周边等分配置。原料的注射可以是朝等离子体气体流中心呈径向，或者有相当大切向和/或轴向的分量流(component)进入等离子体气体流外部区或反应区，用来产生涡流状流动。将注射量调节至所需的反应温度，这取决于热等离子体气体的流动和原料性质。优选的范围是等离子体气体中1-10kWh，以原料中每1千克的碳计。
当此方法不用氧气进行时，反应产物具有特别良好的质量。
在本发明方法的一个实例中，制得有用的产物：炭黑和氢气。本发明的方法能制备多种产物。
本发明方法优选是在一个用来将含碳原料在等离子体内转变为具有清晰纳米结构的碳化合物的反应器中进行，该反应器包括一个室，该室具有
(a)头部，该头部包括至少两根电极和等离子体气体源，用来当施加足够电能时在电极之间产生电弧，从而产生弧区，
(b)文丘里管部分，
(c)反应室，包括至少一个原料注射器，
所述文丘里管部分位于弧区和原料注射器之间，朝反应室方向变窄。
所述反应器较好是圆柱形的。所述室本身，至少是其内表面宜由含石墨的材料制得。
在用本发明方法制备纳米结构的碳材料时，发明人发现反应产物的结构和质量完全取决于工艺参数，主要是反应温度和停留时间，但是与原料关系不大，这一点出乎意料。这也就是为何即便是甲烷或废油都可用来产生具有清晰纳米结构的高质量碳材料的原因。
本发明还提供了一种新炭黑。该炭黑的特征是在氮吸附法表面积(nitrogensurface area)和CTAB表面积之间有负差(通常被称作“孔隙率”)，固有密度(intrinsic density)低于1.9，较好是低于1.8，特别好是1.5-1.9g/cm3。即，
N2SA＜CTAB SA
特别是：
-20m2/g≤N2SA-CTAB SA＜0m2/g。
优选是，炭黑的氮吸附法表面积为5-100m2/g，DBP吸收量为30-300毫升/100克。
此新炭黑的优点是密度低。这在例如轮胎用途中，使得炭黑的所需重量减少，从而使得最终橡胶产品的总重量减少。此新炭黑的另一个用途是作为干电池电极。
本文所述和所说明的炭黑的各种性能用以下标准方法测得。
氮吸附法表面积(N2SA)      ASTM D3037-93
CTAB SA                    ASTM D3765-92
DPB吸收                    ASTM D2414-93
CDBP吸收量                 ASTM D3493
用二甲苯测得的固有密度     DIN 12797
                           (2.5克炭黑，15乇)
碘值                       ASTM D1510
硫含量                     ASTM D1619
灰分含量                   ASTM D1506
pH                         ASTM D1512
甲苯褪色                   ASTM D1618
下文结合附图说明本发明的一些优选特征和实施方案。
图1至图2示出了本发明反应器的一个优选实施方案。
图1是进行本发明方法的一套完整反应器的示意图，
图2是图1反应器上部的详细视图。
图1示出反应器1，该反应器包括圆柱形反应室2，其内壁用石墨制得。反应器的头部3形成了反应器上端。三根电极8位于头部3，与能输出三相交流电的电源4连接。电流频率可以是电网频率(50-60Hz)或者任何更高的频率。反应室2的下端与提取装置5连接，通过该提取装置从反应器中取出反应产物。这些反应产物输入到标准的分离装置6(例如旋风分离器和/或过滤器)中，在该分离装置中炭黑与氢和其它反应产物分离。
反应室2上部更详细的视图见图2。使等离子体气体(优选是氢气、氮气、一氧化碳、氩气或者它们的混合气体)由入口7经过头部3的中央加入到反应室2中。根据等离子体气体的性质和电功率，将等离子体气体流量在每kW电功率0.001至0.3Nm3·h-1之间调节。将连接在电源4上的三根石墨电极8(图2中示出两根)安放在头部3。这些电极的尖端足够靠近在一起，使得当足够的电源与电极连接时，在等离子体气体的存在下能触发复合电弧。结果在弧区9内产生等离子体。该等离子体的温度通过等离子体气体流量和施加到电极8上的电功率来控制。弧区可以通过开孔15用光学高温计来检测。这样就能自动控制流入反应区的等离子体气体的温度和/或量。
在弧区9下方，用石墨制得的文丘里管部件11位于反应器1的内部。当等离子体气体流经过文丘里管部件11的窄通道即喉部20时其速度增加。
等离子体气体在经过文丘里管部件11之后突然扩张进入反应区10，文丘里管的下端成形为陡的边缘(sharp edge)而不是连续加宽的段(continuouswidening section)。用注射器13将原料注入反应区10，注射器13位于反应室2的壁12内，文丘里管11的正下方。在文丘里管之后注入原料有助于等离子体气体和原料之间的混合。
优选是，通过2个至5个注射器13将原料正对着反应区10的中央注入或者朝着反应区10的中央径向注入。原料也可以以朝接近相切的方向注入，使得原料偏心地进入反应区10，或者与流动方向同向或逆向成一定角度地进入反应区10。
需要控制的能量视反应过程、原料的流量和性质而定，能量可以通过等离子体气体温度和/或等离子体气体流量和通过电源4施加到电极8上的电功率来控制。
压力优选是稍高于大气压力，以防氧气的泄漏进入。当输入能量(等离子体流加上电功率)足够高时，碳的产率甚至可以达到100％。可通过注入少量碱性盐来减少炭黑结构。通常还可以使用淬冷区，该区中可加入诸如甲烷或其它合适的淬冷材料。
在不注入氧气的情况下进行本发明过程，除了可以将含碳材料转变为具有清晰纳米结构的碳以外，高质量的氢气也是有用的反应产物。因而还可以分离氢气。在设想生产碳化合物(具体是炭黑)和生产氢气时，甲烷或天然气是特别有吸引力的原料。可用的原料例如还有乙烷、乙烯、丙烷、丙烯、丁烷和丁烯。
以下一些实施例中将说明本发明的较佳特点、这些特点的组合以及实施方案。
这些实施例在一套基本上如图1和图2所示的反应器中进行。用等离子体电源向三根石墨电极供电，该等离子体电源使用高达666Hz的三相电源，其最大功率为263kVA，电流范围最大为400A，所述三根石墨电极的末端位于等腰三角形的顶点上。
实施例1
在所述反应器中，以9Nm3·h-1的氮气流产生等离子体，该等离子体的工作电流为200A。使用流量为2kg·h-1的裂解燃料油作为烃原料。将该裂解燃料油(PFO)与来自处于0.75-1巴压力下的储罐中的压力为0.5巴的氩气载气一起加入反应器中。注射器位于石墨反应器壁内2厘米处。
用初级过滤器和次级过滤器取出形成的炭黑。
实施例2
在本实施例中，用0.56Nm3·h-1的乙烯作为原料。所用的等离子体还是9Nm3·h-1的氮气，在200A条件下产生的等离子体。注入原料的周期为5分钟，在过滤器中获得290克炭黑。
实施例3
在本实施例中，反应条件与先前一个实施例相同，不同的是以0.56Nm3/h的流量连续注入乙烯30分钟。
实施例4
本实施例的工艺条件相当于先前实施例。在本实施例中，以0.56Nm3·h- 1的流量注入乙烯16分钟。等离子体气流是9Nm3·h-1的氮气。
实施例5
本实施例的工艺条件相当于先前实施例。在本实施例中，以0.6Nm3·h-1的流量注入甲烷90分钟。等离子体气流是12Nm3·h-1的氮气，电流为250A。
按照实施例1-5得到的炭黑，测试其常规性能，结果示于表1。在所有实施例中，碳产率高，例如通过调节能量和原料流总可能达到100％。
                              表1：炭黑性能
  实施例1   实施例2   实施例3   实施例4  实施例5
  BET(m2/g)     69     75.1     74.6     76     69
  CTAB(m2/g)     95.7     90.9
  I2(m2/g)     95.2     91.9
  DBP(ml/100g)     218     210     224     206     221
  CDBP(ml/100g)     94     125     124     127     121
  pH     7.5     8.98     8.96     8.86     7.76
  灰分(％)     0.08     0.32     0.28
  C-产率     100     80      75     85     60
  甲苯褪色(％)     72      80     87
  硫     0.04     0.036      0.074
此外，用本发明装置按本发明方法获得的本发明炭黑进行了在标准橡胶组合物ASTM 3191和典型电池电极用途中的试验。表2至表6示出了这些试验获得的数据。
炭黑IRB#7、N-234和Ensaco 250是标准炭黑，下表中也示出了这些炭黑的性能用来与本发明炭黑进行比较。本发明炭黑以实施例A至D表示，其中实施例D的炭黑与表1中实施例1的炭黑相同。实施例A至C的炭黑用略有不同的工艺条件获得。
                                     表2
炭黑  IRB#7N-234 Ensaco 250 实施例A 实施例B 实施例C 实施例D(等于表1中实施例1)
方法 炉法 MMM 等离子体 等离子体 等离子体 等离子体
原料 滗析油，PFO，煤焦油 PFO CH4 C8H8 C2H4 PFO
                                        表3
炭黑   IRB#7   N-234  Ensaco 250 实施例A 实施例B 实施例C 实施例D
氮吸附法表面积(m2/g)    80    125     65    65    52    80    69
DBP吸收量(ml/100g)   102    125     190    157    153    232    218
粘度和流变数据
                                           表4
炭黑   IRB#7   N-234  Ensaco250  实施例A   实施例B   实施例C   实施例D
ML1+4，100℃   83.6   98.3   103.4     85     73.4     107
                                      流变仪，于160℃
最小扭矩(dNm)   2.91   3.71   4.11     3.03     2.36     4.34     2.77
最大扭矩(dNm)   21.27   26.62   23.42     22.61     19.48     26.59     22.37
Δ扭矩(dNm)   18.36   22.91   19.31     19.58     17.12     22.25     19.60
T90(分钟)   14.5   14.96   20     9.34     15.56     9.57     14.21
                                            表5
炭黑   IRB#7   N-234   Ensaco250   实施例A   实施例B   实施例C   实施例D
                              在S2上的应力应变，500mm/min
拉伸强度，Mpa     28.5   31.5     25     23.8     20.4     24.7     21.4
模量100％(MPa)     3.6   3.5     3.3     3.3     2.6     3.9     3.2
模量200％(MPa)     10.5   10.3     7.9     8.7     6.4     9.8     7.8
模量300％(MPa)     19.4   19.8     12.8     14.8     10.9     15.9     13.1
断裂伸长率(％)     426   443     571     490     551     508     499
肖氏硬度A     70    72      70      69     64      73     67
回弹(％)   46.2   41.4    41    47.4     51.3    42.9     51.8
电阻率(欧姆·厘米)   600.103   240.103    12.5    1.4103     106    165.103
                              表6
电池评定*   炭黑-实施例4  电池炭黑-Super P
开路电压(V)     1.652     1.654
短路电流(A)     9     10.7
达到1.1V的时间(小时)     7.42     8.53
达到0.9V的时间(小时)     11.63     12.63
*R20型电池具有以下组成：
-MnO2-         50.73％
-NH4Cl-         1.92％
-炭黑-          10.79％
-ZnO-           0.64％
-ZnCl2-         9.72％
-H2O-           26.63％
-HgCl2-         0.03％

Claims (10)

1.一种通过转变含碳原料制造炭黑或含碳化合物的方法，该方法包括以下步骤：
·用电能产生等离子体气体，
·引导所述等离子体气体经过文丘里管，该管的直径沿等离子体气体流
  动方向变窄，
·将所述等离子体气体导入反应区，在反应区占优势的空气动力和电磁
  力产生的流动条件下，原料或产物未明显地发生再循环进入等离子体
  产生区的现象，
·在反应区中将原料注入等离子体气体，
·从反应区回收反应产物，
·将炭黑或含碳化合物与其它反应产物分离。
2.如权利要求1所述的方法，其特征在于通过引导等离子体气体经过电弧，较好是至少三根电极产生的复合电弧，来产生所述等离子体气体。
3.如权利要求1或2所述的方法，其特征在于该方法还具有以下特征中的一个或多个：
(a)用包含石墨的电极产生等离子体；
(b)通过在电极上连接交流电源来产生电弧；
(c)电流频率在50Hz至10kHz之间；
(d)文丘里管在其内表面包含石墨；
(e)文丘里管的形状是连续的分级锥形；
(f)所用的文丘里管的出口端从文丘里管的喉部陡然扩张；
(g)原料选自以下物质的一种或多种：甲烷、乙烷、乙烯、乙炔、丙烷、丙烯、重油、废油、裂解燃料油，所述原料可以与载气一起加入，也可以不用载气加入，可以经预热后加入，也可以不经预热加入；
(h)原料是一种固态碳材料，与载气一同注入，所述固态碳材料选自以下物质的一种或多种：炭黑、乙炔黑、热炭黑石墨、焦炭或任何固态碳材料；
(i)向所述原料中加入金属催化剂，较好是Ni、Co、Fe；
(j)将所述等离子体气体从电极中央上方沿轴向注入，为的是正好通过弧区中的电弧；
(k)产生所述等离子体气体的气体包含以下物质中的一种或多种或者由其组成：氢气、氮气、氩气、一氧化碳、氦气；
(l)所述原料是烃，所述反应区中的温度在900℃至3000℃之间；
(m)所述原料是固态碳，所述反应区中的温度在3000℃至5000℃之间；
(n)按照所述等离子体气体的性质和电功率，在每kW电功率0.001Nm3/h至0.3Nm3/h之间调节等离子体气体的流量；
(o)将反应尾气的一部分再循环，作为用来产生等离子体气体的至少一部分气体；
(p)将所述原料通过至少一个注射器，较好是2个至5个注射器注入；
(q)将所述原料朝着所述等离子体气体流的中央注入；
(r)将所述原料以切向和/或径向和/或轴向分量流进入所述等离子体气体流外部区的方式注入；
(s)该方法在不存在氧气的情况下进行，或者有少量氧气存在的情况下进行，较好是氧/碳的原子量比小于1/6；
(t)该方法在外加碱的存在条件下进行，以减少结构；
(u)回收下列一种或多种产物：
- 炭黑；
- 富勒烯；
- 氢；
- 单壁纳米管；
- 多壁纳米管。
4.一种实施方法权利要求之一所述方法的装置，该装置包括流体连通的以下部件：
·头部(3)，包含
- 至少两根电极(8)，和
- 气体源，
用于当施加足够电功率时在电极之间产生电弧从而产生弧区，来自气体源的气体可加入该弧区中产生等离子体气体，
·文丘里管形状的限制管(11)
·反应段(10)，和
至少一个原料注射器(3)，用于将原料气体注射进入反应区，
所述文丘里管朝反应段方向变窄。
5.如权利要求4所述的反应器，其特征在于所述反应器大致为内部圆柱形。
6.如权利要求4或5所述的反应器，其特征在于所述暴露于高温的表面用含石墨的耐高温材料制得。
7.如权利要求4、5或6所述的反应器，其特征在于该反应器包括高度为1.5-5米、直径为20-150厘米的室。
8.一种炭黑，它在氮吸附法表面积和CTAB表面积之间有负差，其固有密度小于1.9g/cm3，较好为1.5-1.8g/cm3。
9.如权利要求8所述的炭黑，其特征在于其氮吸附法表面积为5-150m2/g，其DBP吸收量为30-300ml/100g。
10.如权利要求8或9所述的炭黑，其特征在于该炭黑的孔隙率确定在以下范围内：
-20m2/g≤N2SA-CTAB SA＜0m2/g。
CN01815791A 2000-09-19 2001-09-19 将含碳原料转变为有清晰纳米结构含碳材料的装置和方法 Pending CN1458966A (zh)

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