CN101023243A - 烧结球形颗粒 - Google Patents

烧结球形颗粒 Download PDF

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Publication number
CN101023243A
CN101023243A CNA2005800306603A CN200580030660A CN101023243A CN 101023243 A CN101023243 A CN 101023243A CN A2005800306603 A CNA2005800306603 A CN A2005800306603A CN 200580030660 A CN200580030660 A CN 200580030660A CN 101023243 A CN101023243 A CN 101023243A
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China
Prior art keywords
weight
proppant
sintering aid
composition
bauxite
Prior art date
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CNA2005800306603A
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English (en)
Inventor
R·迪恩克尔
M·埃蒙兹
S·卡诺瓦
B·埃尔德雷德
B·A·威尔逊
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Carbo Ceramics Inc
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Carbo Ceramics Inc
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Publication of CN101023243A publication Critical patent/CN101023243A/zh
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Abstract

描述了包含氧化铝微粒、粘土和铝土矿中至少一种和任选的烧结助剂的烧结、球形复合颗粒或微粒以及它们的制造方法。同时还描述了这种颗粒在液压破裂地下岩层与研磨中的用途。

Description

烧结球形颗粒
发明背景
本发明涉及石油天然气井支撑剂，更确切地说，涉及在宽范围应用中显示优异的耐磨性的支撑剂，其中用于生产该支撑剂的原料之一是氧化铝微粒。
石油和天然气由具有多孔且可渗透地下岩层的井产生。岩层的多孔性允许该岩层储存石油和天然气，而且岩层的渗透性允许石油或天然气流体穿过岩层移动。岩层的渗透性对于允许石油和天然气流动到其能够从井泵送的场所是关键。某些情况下，蕴藏天然气和石油的岩层的渗透性不足以经济地回收石油和天然气。其它情况下，在井的操作期间，岩层的渗透性下降到进一步回收变得不经济的程度。在这样的情况下，必须破碎岩层并且在开放条件下利用支撑材料或支撑剂支撑破碎。这样破碎通常利用水压完成，支撑材料或支撑剂是粒状材料，例如砂、玻璃珠或陶瓷球，其通过流体被带入裂缝。
尺寸均匀的球形颗粒被普遍公认为是最有效的支撑剂，因为其渗透性最佳。为此，假定其它的性能相同，球形或基本球形的支撑剂，例如圆形砂粒、金属丸、玻璃珠、金刚砂或机械加工为球形的其它陶瓷材料是优选的。
发明详述
依照本发明，生产了具有作为起始原料之一的氧化铝微粒的球形丸粒或颗粒。该球形颗粒适合用作石油和天然气支撑剂以及研磨介质。该球形微粒在烧结温度下烧充分长的时间，以能够获得表观比重为2.70-3.75g/cm3且堆积密度为约1.35-约2.15g/cm3的烧结的球形颗粒。本发明实施方案的支撑剂在从中等到异常高强度范围内变化并且在高达约15,000psi闭合应力(closure stress)下有效。因而，本发明实施方案的支撑剂通常可应用于闭合应力极端的中等深度或非常深的石油和天然气井。
球形颗粒由氧化铝微粒与粘土和铝土矿中的至少一种的组合物制备。另外，所述组合物中可以加入烧结助剂。合适的烧结助剂包括氧化铁和氧化锌。所述组合物可以包含约10-75重量％氧化铝微粒、约20-90重量％粘土和铝土矿中的至少一种，和，任选地，约0.1-15重量％烧结助剂。粘土和铝土矿可以包含约35-90重量％氧化铝。在一种实施方案中，所述组合物包含58重量％氧化铝微粒和42重量％煅烧高岭土。在另一种实施方案中，所述组合物包含64重量％氧化铝微粒、28重量％高岭土和8重量％氧化铁。在另一种实施方案中，所述组合物包含20重量％氧化铝微粒和80重量％铝土矿。在另外一种实施方案中，所述组合物包含36重量％氧化铝微粒、63重量％铝土矿和1重量％氧化锌。
适合在生产本发明实施方案支撑剂的组合物中应用的氧化铝微粒材料是采用拜耳法的净化氧化铝的氧化铝微尘收集器的副产物。依照拜耳法，将铝土矿的铝成分溶于氢氧化钠，从该溶液中除去杂质并且从该溶液沉淀三水合氧化铝，然后煅烧为氧化铝。拜耳法设备主要是一种加热并冷却大量循环的苛性钠溶液物流的装置。铝土矿在高温点加入，红泥在中等温度下分离，氧化铝则在该循环的低温点沉淀。适合制备本发明实施方案支撑剂颗粒的氧化铝微粒是该方法的副产物。合适的氧化铝微粒产物的氧化铝含量为约99重量％，烧失量为约13％-22％，平均粒径为约12微米并且约86％或更高的粒径分布小于45微米。术语“烧失量(loss on ignition)”指本领域普通技术人员公知的一种方法，其中试样在约100℃干燥以驱除游离水分，然后加热到约1000℃以驱除化学结合水和其它化合物。
用于生产本发明实施方案支撑剂的组合物还包含粘土和铝土矿中的至少一种。对生产本发明实施方案支撑剂的组合物合适的粘土材料是高岭土。自然界发现的高岭土是水合硅酸铝，其组成为约52％SiO2和45％Al2O3(所述的化学成分以基于煅烧的重量百分比表示)。合适的高岭土开采于Mclntyre，Georgia地区并且具有大约14％的烧失量。根据某些实施方案，所述高岭土材料可以使用本领域普通技术人员公知的方法在除去足够水化水的温度和时间下煅烧以促进粒化。
对生产本发明上述方式支撑剂的组合物合适的铝土矿材料可由Comalco获得。自然界可见的这种铝土矿具有的化学组成为大约82％Al2O3、7％SiO2(所述的化学成分以基于煅烧的重量百分比表示)。所述铝土矿从澳大利亚开采且煅烧，认为自始具有大约低于1％的烧失量。根据某些实施方案，所述铝土矿材料可以使用本领域普通技术人员公知的方法在除去足够水化水的温度和时间下煅烧以促进粒化。
应用于生产本发明实施方案支撑剂组合物的粘土和铝土矿材料与多种支撑材料是相容的并且可作为其基质使用，因此依照该方式，可以生产多种复合支撑剂，其可以根据具体的条件或岩层定制。因而，最后烧结的复合材料颗粒的性能，例如强度、渗透性、表观比重、堆积密度和耐酸性，可通过初始组分混合物的变化得到控制。
此外，球形颗粒可定制用作研磨介质。例如，通过适当选择起始材料、尤其是特殊的烧结助剂可使研磨介质达到期望的颜色和密度。研磨介质常常要求浅颜色以使介质在研磨期间的磨耗不会污染被研磨的产物。在这种情况下，烧结助剂如氧化铁不会使用，原因在于氧化铁存在使介质变黑的趋势。相反，烧结助剂如氧化锌可以使用，因为其产生浅颜色介质。通过调整起始材料的相对比例可以获得期望密度的研磨介质。例如，包含较大量氧化铝微粒或铝土矿的起始成分的比率将导致形成较高密度的介质。较高密度的研磨介质提高了球磨机和立磨机的研磨能力。合适的研磨介质性能如耐摩性同样为本领域普通技术人员公知。
正如这里所用，术语“表观比重”是无单位的数值，但是定义为数值上等于每立方厘米体积的重量，在体积确定中排除空穴体积或开放孔隙。这里给出的表观比重值通过水置换确定。
正如这里所用，术语“堆积密度”定义为单位体积的平均重量，包括颗粒之间的空穴体积。
除非另有说明，关于组合物的所有百分比、比例和值均以重量表示。
如上所述，生产本发明实施方案支撑剂的组合物还可以包含烧结助剂，例如氧化铁或氧化锌。氧化铁可以赤铁矿氧化铁(Fe2O3)或其它形式的氧化铁如FeO和Fe3O4加入所述组合物，因此这里使用的所有术语″氧化铁″意味着所有形式的氧化铁并且可统称为FexOy。合适的氧化铁材料是可由Densimix，Inc商业获得的颜料级氧化铁。合适的氧化锌材料可由U.S.Zinc商业获得。
本发明还提供一种利用本发明实施方案支撑剂以高达20,000英尺深度支撑石油和天然气井中裂缝的方法，该方法将支撑剂与流体如油或水混合，并且将该混合物引入地下岩层的裂缝。作用于裂缝上的挤压压力通常最高约15,000psi。
在本发明实施方案的方法中，氧化铝微粒、粘土和铝土矿中的至少一种和任选的一种或多种烧结助剂的组合物被研磨为精细颗粒大小的粉尘。将该粉尘混合物加入具有可转动工作台的高强度混合器内，其中的工作台装配有可转动撞击叶轮，例如在授予Brunner的美国专利No.3,690,622中所述。加入充足的水以形成基本球形的陶瓷颗粒。任选地，粘结剂，例如现有技术公知的各种树脂或蜡、淀粉或聚乙烯醇可以加入初始混合物中以改进粒化过程并且提高未烧结颗粒的生坯强度。合适的粘结剂为淀粉，其可以约0-1.5重量％的水平添加。在某些实施方案中，淀粉可以约0.5-0.7重量％的量加入。
所获得的颗粒然后干燥并且筛分到适当的预烧结尺寸，并且在烧结温度下烧直到获得约2.70-约3.75的表观比重，这取决于起始混合物的组成。
本领域普通技术人员认为所述组合物还可以包含其它的传统烧结助剂，其中包括，例如，微量的膨润土、长石、霞石正长岩、滑石、氧化钛，和锂、镁、钾、钙、锰和硼的化合物，例如碳酸锂、氧化钠、碳酸钠、硅酸钠、氧化镁、碳酸镁、氧化钙、碳酸钙、氧化锰、硼酸、碳化硼、二硼化铝、氮化硼和磷化硼。最期望的烧结助剂范围可容易地由本领域熟练技术人员根据具体使用的氧化铝微粒、粘土和铝土矿的混合物确定。
本发明实施方案的烧结支撑剂颗粒是球形的。所述支撑剂颗粒球形度利用视觉比较器确定。Krumbein和Sloss在Stratigraphy andSedimentation，第二版，1955，W.H.Freeman&Co.，San Francisco，Calif.，描述了用于视觉确定球形度和圆度的图表。利用该图表的视觉比较是一种广泛使用的评价颗粒球形度或圆度的方法。在利用该视觉比较的方法中，随机选择20种要测试材料的颗粒试样。在10-20倍的显微镜或显微镜照片下观察这些颗粒并将其形状与Krumbein和Sloss图表比较。该图表的球形度值范围为0.3-0.9。然后平均各个颗粒的图表值获得球形度值。
正如这里所用，术语“球形”和有关形式定义为最小直径与最大直径的平均比例为约0.80或更高，或与Krumbein和Sloss图表相比具有的平均球形度为约0.8或更高。当与Krumbein和Sloss图表视觉比较时，本发明实施方案的烧结支撑剂颗粒具有的平均球形度为约0.8或更高。本发明某种实施方案的支撑剂颗粒具有约0.9的圆度和约0.9的球形度。
生产本发明实施方案的烧结、球形颗粒的合适步骤如下：
1.将氧化铝微粒、粘土和铝土矿中的至少一种，任选的一种或多种烧结助剂，和任选的粘结剂的初始成分研磨到其中约90-100％小于325目。根据某些实施方案，煅烧粘土和铝土矿中的一种或两者，并且如果存在的话，粘结剂为淀粉。将90重量％的磨细起始成分加入高强混合器内。
2.用合适的商业可得的搅拌或混合装置搅拌起始成分，其中搅拌或混合装置具有可转动的水平或倾斜圆形工作台和可转动的撞击叶轮。
3.在搅拌混合物的同时，加入足量的水以促使球形颗粒形成和使这些颗粒长大到期望尺寸。
总之，足以促使形成基本球形颗粒的水的总量为起始成分的约17-约23重量％。总混合时间通常为约2-约15分钟。
在氧化铝微粒、粘土和铝土矿的至少一种、任选的一种或多种烧结助剂和任选粘结剂的化合物已经长大为期望尺寸的球形颗粒后，降低混合器的速率，并且将10重量％的磨细起始成分加入混合器。
4.干燥获得的颗粒并筛分至规定尺寸，该规定尺寸将补偿在窑炉烧结期间出现的收缩。优选在干燥后对颗粒进行尺寸筛分。在干燥和筛分步骤后获得的拒绝的过大和过小颗粒与粉末材料可以再循环。
5.然后干燥后的颗粒在烧结温度下烧足够长的时间以能够获得烧结的、表观密度为2.70-3.75且堆积密度为约1.35-约2.15g/cm3球形颗粒。具体采用的时间和温度取决于起始成分并且根据烧后的物理试验结果经验地确定。
还可以在烧后筛分颗粒。最终的颗粒可进行磨光处理以增强光滑度。本发明实施方案支撑剂具有符合20/40支撑剂API规定的粒径分布，其规定所述产物必须在初次20-40目筛分之间保留90％。但是，使用相同的混合物还可以生产140目-6目之间的其它尺寸支撑剂。依照本发明实施方案制备的支撑剂显示了下列典型筛分分析(保留的重量％)：
U.S.目 微米  20/40
+16 +1180  0
-16+20 -1000+850  3
-20+30 -850+600  69
-30+40 -600+425  27
-40 -425  0
表I报道的堆积密度利用步骤ANSI B74.4通过称量用于填充已知体积杯子的试样量确定。
表I报道的破碎值利用美国石油组织(API)用于确定破碎阻力的步骤获得。依照该步骤，将约6mm厚的要测试试样床放置在空心圆筒单元内。将活塞塞入该单元内。然后，通过活塞向试样施加荷载。用时1分钟达到最大负荷并且保持该负荷2分钟。然后除去负荷，从单元内取出试样并且筛分分离破碎的材料。结果以破碎到小于起始材料尺寸的材料占原始试样的重量百分比表示(例如，20/40材料将为破碎到-40目的材料)。
表I对由所述原料生产的颗粒的本发明实施方案组合物进行了总结。同时还给出了这些颗粒的试验结果。所有试样依照这里描述的步骤制备。实施例1-4对表I报道的受测支撑剂试样制备中采用的步骤作了详细描述。
混合物的化学组成由原料混合比计算，并且通过本领域普通技术人员公知的分析方法-感应耦合等离子体(ICP)测定原料的化学组成。
表I
    化学成分     氧化铝微粒     氧化铝/高岭土(58∶42)    氧化铝/高岭土/氧化铁(64∶28∶8) 氧化铝/铝土矿/ZnO(36∶63∶1)     氧化铝/铝土矿(20∶80)
    Al2O3     98.77     77.18    77.96 89.8     85.6
    Fe2O3     0.03     0.43    7.95 0.7     5.4
    K2O     0     0.04    0.02 0.1     0.01
    SiO2     0.08     21.31    12.57 4.9     5.7
    CaO     0.04     0.1    0.09 0.2     0.02
    NaO     1.07     N/A    0.74 0.4     0.2
    MgO     0     0.04    0.02 0.1     0.02
    P2O5     0     0.04    0.01 0.1     0.01
    TiO2     0     0.86    0.57 2.4     2.9
    ZnO     0     0    0 1.0     0
    LOI     15.6     13.4    12.4 14.9     4.2
    20/40性能
    BD     1.34    1.84 1.99     1.98
    ASG     N/A    3.3 3.65     3.63
    15,000psi/破碎 7.4     2.9
    10,000psi/破碎    2.9
    4,000psi/破碎     2.1
    球形度     ＞0.8    ＞0.8 ＞0.8     ＞0.8
实施例1
比例为58/42的氧化铝微粒与煅烧高岭土的混合物首先进行研磨处理以使该混合物的99.4％具有小于325目的粒径。接着，将约3200g比例为58/42的混合物装入R02 Eirich混合器。
该混合器以高转速操作并且加入1050g其中包含24g作为粘结剂的淀粉的水。粒化过程以高速持续4.5分钟。然后，将混合器的转速降低到“慢”转速并加入200g同样具有58/42比例的氧化铝微粒与煅烧高岭土的组合物的研磨粉末。颗粒在慢转子作用下研磨总计1.5分钟。
然后在于2850-3000温度下烧之前干燥颗粒并且筛分为-16目/+30目。所获得的颗粒具有堆积密度1.34gm/cm3。
所述颗粒的破碎强度依照API步骤测试以测定在4,000psi施加压力下的上述抗破碎能力，所述颗粒具有的破碎百分率为2.1。在实验室窑炉的最大温度能力3000下获得最好强度。数据表明在较高温度下由该混合物烧结的颗粒能够产生具有最佳强度的颗粒。
实施例2
将约3200g比例为64/28/8且98.6％的粒径＜325目的氧化铝微粒、煅烧高岭土和氧化铁混合物装入R02 Eirich混合器。
高速操作该混合器并且加入750g其中包含24g淀粉粘结剂的水，其中的淀粉粘结剂可以商品名Staramic 100由Tate and Lyle NorthAmerica获得。持续旋转工作台和叶轮约10.5分钟；接着，降低叶轮速度并且添加200g比例同样为64/28/8的氧化铝微粒、煅烧高岭土和氧化铁组合物的研磨粉末。研磨持续大约2分钟。
然后在于约2,750温度下烧之前干燥颗粒并且筛分为-16目/+30目。所获得的颗粒具有表观比重约3.30、堆积密度1.84gm/cm3、球形度大于0.8，所述值利用Krumbein和Sloss图表测定。
所述颗粒的破碎强度依照API步骤测试以测定在10,000psi施加压力下的上述抗破碎能力，所述颗粒具有的破碎百分率为2.9，符合API关于该尺寸的支撑剂最大破碎比例10％的规定。
实施例3
将约4.5kg比例为36/63/1且99.9％粒径＜325目的氧化铝微粒、铝土矿和氧化锌混合物加入R02 Eirich混合器。
高速操作该混合器并且加入约1000g水。持续旋转工作台和叶轮约6分钟；接着，降低叶轮速度并且添加约450g比例同样为36/63/1的氧化铝微粒、铝土矿和氧化锌的组合物研磨粉磨。研磨持续大约1分钟。
然后在于约2,840温度下烧之前干燥颗粒并且筛分为-16目/+30目。所获得的颗粒具有表观比重约3.65、堆积密度1.99gm/cm3、球形度大于0.8，所述值利用Krumbein和Sloss图表测定。
所述颗粒的破碎强度依照API步骤测试以测定在15,000psi施加压力下的上述抗破碎能力，所述颗粒具有的破碎百分率为7.4，符合API关于该尺寸的支撑剂最大破碎比例10％的规定。
实施例4
将约3.6kg比例为20/80且99.9％的粒径＜325目的氧化铝微粒与铝土矿的混合物加入R02 Eirich混合器。
高速操作该混合器并且加入约800g水。持续旋转工作台和叶轮约6分钟；接着，降低叶轮速度并且添加约360g比例同样为20/80的氧化铝微粒与铝土矿组合物的研磨粉末。研磨持续大约1分钟。
然后在于约2,750温度下烧之前干燥颗粒并且筛分为-16目/+30目。所获得的颗粒具有表观比重约3.63、堆积密度1.98gm/cm3、球形度大于0.8，所述值利用Krumbein和Sloss图表测定。
所述颗粒的破碎强度依照API步骤测试以测定在上述破碎和15,000psi施加压力下的抗破碎能力，所述颗粒具有的破碎百分率为2.9，符合API关于该尺寸的支撑剂最大破碎比例10％的规定。
本发明球形、烧结颗粒适合在破裂地下岩层方法中用作支撑剂以提高其渗透能力，特别是通常位于深度达约20,000英尺的挤压压力约15,000psi的岩层的渗透能力。
当用作支撑剂时，本发明颗粒可按照与其它支撑剂相同的方式处理。所述颗粒可以袋装或散装形式随破碎处理使用的其它材料一起输送到井现场。传统设备和技术可用于放置作为支撑剂的球形颗粒。
经常称为“前置液体”的粘性流体以引发并促进地下岩层破裂的速度注入井。破碎液体可以是油基、水基、酸、乳液或任何其它流体。破碎液体的注射持续进行直到获得充分的几何破裂以允许置换支撑颗粒。然后，通过将所述颗粒已经预先引入并悬浮其中的流体注入裂缝将上述颗粒放入裂缝。支撑分布通常为，但是不必要，多层填充。在放置所述颗粒之后，将该井关闭足够长时间以允许裂缝内压力释放进入岩层内。这样导致裂缝闭合并且抵抗裂缝进一步闭合的支撑颗粒施加压力。
另外，本发明球形、烧结颗粒适合用作研磨介质。当用作研磨介质时，颗粒接近白色或淡褐色，这是用于矿石研磨或其它类型的研磨产品颜色为关键质量参数的研磨的介质需要的性能。当本发明球形、烧结颗粒在使用过程中完全磨损时，它们不会产生在使用金属介质或深色陶瓷介质情况下出现的产品变色的情况。
前文的说明和实施方案旨在说明本发明，并不对其构成任何限制。应该理解不脱离本发明精神和范围可以进行任何改进。

Claims (36)

1.一种包含大量烧结的球形颗粒的天然气与石油井支撑剂，所述颗粒由包含氧化铝微粒和粘土与铝土矿至少之一的组合物制备。
2.如权利要求1所述的支撑剂，其中所述组合物进一步包含至少一种烧结助剂。
3.如权利要求2所述的支撑剂，其中至少一种烧结助剂选自氧化铁、氧化锌、膨润土、长石、霞石正长岩、滑石、氧化钛、碳酸锂、氧化钠、碳酸钠、硅酸钠、氧化镁、碳酸镁、氧化钙、碳酸钙、氧化锰、硼酸、碳化硼、二硼化铝、氮化硼和磷化硼。
4.如权利要求2所述的支撑剂，其中所述组合物包含约10-约75重量％氧化铝微粒、约20-约90重量％粘土和铝土矿中的至少一种和约0.1-约15重量％至少一种烧结助剂。
5.如权利要求4所述的支撑剂，其中所述组合物包含约40-约75重量％氧化铝微粒、约20-约60重量％粘土和约0.1-约15重量％至少一种烧结助剂。
6.如权利要求5所述的支撑剂，其中所述组合物包含高岭土。
7.如权利要求6所述的支撑剂，其中所述组合物包含煅烧过的高岭土。
8.如权利要求4所述的支撑剂，其中所述组合物包含约10-约75重量％氧化铝微粒、约20-约90重量％铝土矿和约0.1-约15重量％至少一种烧结助剂。
9.如权利要求1所述的支撑剂，其中所述组合物包含58重量％氧化铝微粒和42重量％粘土。
10.如权利要求2所述的支撑剂，其中所述组合物包含64重量％氧化铝微粒、28重量％粘土和8重量％至少一种烧结助剂。
11.如权利要求10所述的支撑剂，其中所述的至少一种烧结助剂包含氧化铁。
12.如权利要求2所述的支撑剂，其中所述组合物包含36重量％氧化铝微粒、63重量％铝土矿和1重量％至少一种烧结助剂。
13.如权利要求12所述的支撑剂，其中所述的至少一种烧结助剂包含氧化锌。
14.如权利要求1所述的支撑剂，其中所述组合物包含20重量％氧化铝微粒和80重量％铝土矿。
15.如权利要求1所述的支撑剂，其中所述组合物包含高岭土。
16.如权利要求15所述的支撑剂，其中所述组合物包含煅烧过的高岭土。
17.如权利要求1所述的支撑剂，其中所述颗粒具有的表观比重为约2.70-约3.75。
18.如权利要求1所述的支撑剂，其中所述颗粒具有的堆积密度为约1.35-约2.15g/cm3。
19.一种破碎位于深达约20,000英尺深度的地下岩层的方法，其中包括：
以足以打开其中裂缝的速率和压力将液压流体注入所述岩层，并且
将包含烧结球形颗粒的流体注入裂缝，其中所述颗粒由包含氧化铝微粒和粘土与铝土矿中至少一种的组合物制备。
20.如权利要求19所述的方法，其中的组合物进一步包含至少一种烧结助剂。
21.如权利要求20所述的方法，其中所述的至少一种烧结助剂选自氧化铁、氧化锌、膨润土、长石、霞石正长岩、滑石、氧化钛、碳酸锂、氧化钠、碳酸钠、硅酸钠、氧化镁、碳酸镁、氧化钙、碳酸钙、氧化锰、硼酸、碳化硼、二硼化铝、氮化硼和磷化硼。
22.如权利要求20所述的方法，其中所述组合物包含约10-约75重量％氧化铝微粒、约20-约90重量％粘土和铝土矿中的至少一种和约0.1-约15重量％至少一种烧结助剂。
23.如权利要求22所述的方法，其中所述组合物包含约40-约75重量％氧化铝微粒、约20-约60重量％粘土和约0.1-约15重量％至少一种烧结助剂。
24.如权利要求23所述的方法，其中所述组合物包含高岭土。
25.如权利要求24所述的方法，其中所述组合物包含煅烧过的高岭土。
26.如权利要求22所述的方法，其中所述组合物包含约10-约75重量％氧化铝微粒、约20-约90重量％铝土矿和约0.1-约15重量％至少一种烧结助剂。
27.如权利要求19所述的方法，其中所述组合物包含58重量％氧化铝微粒和42重量％粘土。
28.如权利要求20所述的方法，其中所述组合物包含64重量％氧化铝微粒、28重量％粘土和8重量％至少一种烧结助剂。
29.如权利要求28所述的方法，其中所述的至少一种烧结助剂包含氧化铁。
30.如权利要求20所述的方法，其中所述组合物包含36重量％氧化铝微粒、63重量％铝土矿和1重量％至少一种烧结助剂。
31.如权利要求30所述的方法，其中所述的至少一种烧结助剂包含氧化锌。
32.如权利要求19所述的方法，其中所述组合物包含20重量％氧化铝微粒和80重量％铝土矿。
33.如权利要求19所述的方法，其中所述组合物包含高岭土。
34.如权利要求33所述的方法，其中所述组合物包含煅烧过的高岭土。
35.如权利要求19所述的方法，其中所述颗粒具有的表观比重为约2.70-约3.75。
36.如权利要求19所述的方法，其中所述颗粒具有的堆积密度为约1.35-约2.15g/cm3。
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