CN100591781C - 二氧化钛的附聚 - Google Patents

二氧化钛的附聚 Download PDF

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CN100591781C
CN100591781C CN200580009963A CN200580009963A CN100591781C CN 100591781 C CN100591781 C CN 100591781C CN 200580009963 A CN200580009963 A CN 200580009963A CN 200580009963 A CN200580009963 A CN 200580009963A CN 100591781 C CN100591781 C CN 100591781C
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slag
titanium dioxide
tio
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granularity
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CN1957097A (zh
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P·A·博萨
D·贝辛格
B·A·迪潘纳尔
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Kumba Resources Ltd
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Abstract

根据本发明提供一种二氧化钛熔渣粒子的附聚方法，该方法包括提供d50粒度小于106μm的二氧化钛熔渣；混合熔渣粒子与有机粘结剂；和附聚熔渣粒子和有机粘结剂的混合物成d50粒度为106μm-1000μm的附聚粒子。附聚粒子的(TiO2和FeO)/C质量比大于3.4。本发明也涉及这样的附聚熔渣粒子和生产TiO2的氯化物方法，其中使用这样的附聚的二氧化钛熔渣粒子。

Description

二氧化钛的附聚
发明领域
本发明涉及二氧化钛熔渣的附聚。
背景技术
钛广泛已知它作为金属的用途，但钛的主要用途是采用二化钛(TiO2)的形式。TiO2用作油漆，塑料和纸中的白色颜料。
存在两种生产TiO2颜料的商业方法，即硫酸盐方法和氯化物方法。硫酸盐方法包括在浓硫酸中溶解形式为钛矿石(如钛铁矿)或二氧化钛熔渣的原料。然后将包含溶解的TiO2的液体进行水解以得到固体TiO2。在氯化物方法中，将形式为钛矿石或二氧化钛熔渣的原料在高温(例如950-1200℃)下在氯气中流化以生产包括TiCl4的气体。然后将TiCl4从气体选择性冷凝和与氧气在高温下混合以得到TiO2。
硫酸盐方法装置比氯化物方法装置容易操作和监测，和能够使用具有相对低TiO2含量的原料。然而，现代硫酸盐方法装置的资金成本可以高于相同颜料生产能量的氯化物方法装置的资金成本。此外由于使用更不纯的原料和如下事实存在更高体积的要处理和处置的废产物：用于方法的硫酸盐不能容易地回收和循环。因此氯化物方法是更有利的方法和普及性增长。
氯化物方法的一个要求在于原料的粒度规格必须适用于流化床反应器。此粒度典型地为106μm到850μm±5％(按质量计)。
如上所述原料是钛矿石或二氧化钛熔渣。在近来的开发中升级二氧化钛熔渣和然后将升级的熔渣用作原料。
二氧化钛熔渣通常由钛铁矿矿石在电弧炉中的还原生产以形成生铁和二氧化钛富集的熔渣。将这样形成的二氧化钛富集的熔渣以熔融状态铸入杓子，因此生产从几吨到直到四十吨的固体块。在冷却之后，将这些块破碎和然后碾磨到106-850μm的粒度，使它适用于氯化物方法。已经发现在此碾磨工艺期间一些熔渣降低到小于106μm的粒度，使得它对用于氯化物方法来说太细。
二氧化钛熔渣的附聚是本领域已知的。US2,723,903公开了一种方法，其中将含钛材料(包括Sorel类型熔渣，该熔渣包含大约70质量％的TiO2)，焦化煤(也可以加入一些非焦化煤)和含碳粘结剂的密集、压块混合物在竖式炉中氯化。生产尺寸为50.8mm乘50.8mm乘31.8mm的坯块。例示的坯块的预测(TiO2和FeO)/C质量比为0.7-1.3。
US2,805,120公开了与US2,723,903中相似的方法。
US4,117,076和4,187,117公开了含有沥青质焦化煤和合适粘结剂的粒状Sorel熔渣。粒料具有合适的尺寸以用于流化床反应器。这些粒料再次具有高碳含量和例示的粒料典型地具有2-3.2之间的(TiO2和FeO)/C质量比。
已知用于上述坯块和粒料的煤用作粘结剂和还原剂。如果使用高挥发性含量的煤，在附聚物中使用煤的一个缺点可能是强度的下降。
本发明人现在开发了小于106μm的二氧化钛熔渣粒子的附聚的商业可行方法，因此使得它适用于氯化物方法。已经发现附聚物中的碳含量可以降低和仍然提供具有合适强度的附聚物。
发明描述
根据本发明二氧化钛熔渣粒子的附聚方法包括
-提供d50粒度小于106μm的二氧化钛熔渣；
-混合熔渣粒子与有机粘结剂；和
-附聚熔渣粒子和有机粘结剂的混合物成d50粒度为106μm-1000μm的附聚粒子和附聚粒子的(TiO2和FeO)/C质量比大于3.4。
二氧化钛熔渣可以是任何合适的二氧化钛熔渣，但优选它包括粒度小于200μm和优选TiO2含量大于70％(按质量计)，优选大于75％(按质量计)，和更优选大于80质量％的熔渣细粒。二氧化钛熔渣的组成可使它适用于生产TiO2的氯化物方法的流化床反应器。或者，可以处理二氧化钛熔渣以使熔渣适用于该氯化物方法。在本发明的一个实施方案中可以处理二氧化钛熔渣以脱除不希望的化合物和优选增加熔渣的钛浓度。在本发明的一个实施方案中二氧化钛熔渣可以经历磁力分离以脱除不希望的化合物。此处理可以在下述调整大小之前或之后进行。
如果CaO在熔渣中存在，它存在的数量优选小于0.5质量％，优选小于0.3质量％。如果MgO在熔渣中存在，它存在的数量优选小于3质量％，优选小于1.2质量％。
熔渣可以是衍生自海滩沙钛铁矿的熔渣。
本发明的方法也可包括调整二氧化钛熔渣大小到d50粒度小于106μm的步骤。二氧化钛熔渣大小的调整可以通过任何常规方法进行。例如可以考虑筛分。优选粉碎二氧化钛熔渣，更优选碾磨二氧化钛熔渣。优选球磨机，优选干燥球磨机用于碾磨二氧化钛熔渣。
优选熔渣的d80粒度小于75μm，优选d50粒度小于40μm。优选d50粒度是20μm或17μm或甚至更小。相信粒度越细，附聚越好。
可以使用任何合适的有机粘结剂。有机粘结剂可以选自纤维素产物、乳品场废产物(如乳糖和乳清产物)、天然树胶(如瓜耳胶)、淀粉产物(如玉米，马铃薯和小麦淀粉)、淀粉丙烯酸类共聚物、木材相关产物(如半纤维素)及其一种或多种的混合物。优选粘结剂包括淀粉，优选胶凝化淀粉和更优选胶凝化玉米淀粉。已经发现淀粉不仅仅提供足够的粘结强度，而且其使用也不导致附聚产物的不可接受污染。
二氧化钛熔渣和粘结剂可以采用任何合适的比例混合。在淀粉粘结剂的情况下，可以加入1-5％(按质量计)淀粉。优选加入2-3％(按质量计)淀粉和更优选加入约2.5％(按质量计)淀粉。
二氧化钛熔渣和粘结剂可以采用任何合适的方式混合。在本发明的一个实施方案中粘结剂可以在熔渣调整大小的工艺期间加入，因此获得粘结剂和熔渣的混合。在本发明的另一个实施方案中任何合适的混合机，如高速率混合机可用于获得已经调整大小的熔渣和粘结剂的混合。
由于水分含量在附聚中起重要作用，可以采取步骤以在获得附聚之前获得所需的水分水平。在附聚之前的水分含量可以为1-8％(按质量计)。可以采取步骤以向上调节水分含量。
调整大小的熔渣和粘结剂的混合物可以采用任何合适的方式附聚。优选造粒该混合物。造粒可以由任何合适的方式进行，但优选使用盘式造粒机。
优选在造粒工艺期间加入水。加入的水量适于获得可接受的造粒。
优选至少60％(按质量计)，优选至少75％(按质量计)，优选至少90％(按质量计)附聚粒子的尺寸为106-1000μm，优选106-850μm。在本发明的优选实施方案中，附聚粒子的d50粒度为150-1000μm，优选150-850μm。
(TiO2和FeO)/C质量比优选大于4，更优选大于5，和更优选大于10。预见合适的还原剂如碳(例如)可以引入附聚产物，但尽管那样以上比例是有效的。在本发明的优选实施方案中，(TiO2和FeO)/C质量比为优选至少20，优选至少25，优选大于40和甚至大于80。
优选附聚粒子的密度大于1g/cm3，优选大于1.1g/cm3，优选大于1.2g/cm3和更优选大于1.3g/cm3。
形成的附聚粒子/粒料可以经历热处理。在本发明的一个实施方案中可以将附聚粒子/粒料仅干燥，例如在60℃下。或者粒料可以在高温下，典型在约160℃或200℃和甚至250℃下处理以获得粒料的干燥和硬化。
粒料也可以调整大小到106-850μm。可以循环尺寸过大粒料(+850μm)和尺寸不足粒料(-106μm)。
这样形成的粒料或附聚物可适用于生产TiO2的氯化物方法，该方法包括流化床反应器。根据本发明的另一方面提供一种附聚的二氧化钛熔渣粒子，该熔渣粒子含有d50粒度为106-1000μm的附聚粒子，和附聚粒子的(TiO2和FeO)/C质量比大于3.4。优选它包括造粒的二氧化钛熔渣粒子。优选附聚粒子由基本以上所述的方法制备。
根据本发明的另一方面提供生产TiO2的氯化物方法，其中使用上述的附聚的二氧化钛熔渣粒子。氯化物方法可包括如下步骤：
-提供基本如上所述的附聚的二氧化钛熔渣粒子；
-供应附聚的二氧化钛熔渣与还原剂和氯气到流化床反应器中以生产气态四氯化钛；
-冷凝气态四氯化钛；和
-氧化冷凝的四氯化钛以形成TiO2。
附聚的二氧化钛熔渣可以由基本在此以上所述的方法制备。流化床反应器可以在高温下，典型地900-1200℃下操作。合适的还原剂可以是含碳产物。还原剂可以引入附聚的二氧化钛熔渣中。或者，它可以单独提供。在流化床反应器中生产的气态四氯化钛是也包含许多其它氯化物产物的气体流一部分。该气体流通常当它离开流化床反应器时被冷却和然后冷凝。由于各种氯化物产物沸点的差异，四氯化钛产物与其它氯化物产物(如铁氯化物)的分离是可能的。可以将分离的四氯化钛冷却和可以在氧化以形成TiO2之前清洁。然后可进一步加工这样形成的TiO2以生产最终颜料产物。
本发明现在通过如下非限制性实施例进一步描述。
实施例1
三种不同尺寸的熔渣细粒产物从单一高二氧化钛熔渣本体样品(衍生自海滩沙钛铁矿的熔渣)获得用于造粒测试工作。将第一样品(SF1)在球磨机中碾磨到17μm的d50。将第二样品(SF2)在106μm筛上筛分，-106μm尺寸级分用于造粒测试工作。此样品的d50是62μm。第三样品(SF3)是本体样品的代表和如接收时那样使用。此样品的d50是126μm。以下给出本体样品的典型化学组成(表1)：
表1
  SiO<sub>2</sub>(％)   Al<sub>2</sub>O<sub>3</sub>(％)   Fe<sub>总</sub>(％)   TiO<sub>2</sub>(％)   CaO(％)   MgO(％)   MnO(％)   Cr<sub>2</sub>O<sub>3</sub>(％)   V<sub>2</sub>O<sub>5</sub>(％)
  2.52   1.27   8.63   85.2   0.25   1.08   2.00   0.16   0.37
％是质量％
胶凝化玉米淀粉用作所有造粒测试中的粘结剂。对于每个测试，将样品与粘结剂在高强度混合机中在造粒步骤之前混合。盘式造粒机(1.2m直径)用于不同混合物的造粒。在造粒步骤期间向每种混合物中加入足够的水以保证要求粒料的生产。将采用此方式生产的粒料在60℃下干燥。从每个测试，-3+1mm级分筛分出和用于粒料的物理强度测定。对于微粒料强度的测定，使用500g的-3+1mm级分。然后将此样品在轨道震动器上筛分4分钟和确定-0.5mm材料的数量。这用作粒料冷强度的定量测量。来自每个测试的样品(-3+1mm粒料)也在1100℃下在马弗炉中经历高温震荡测试以模拟在向炉中的加载条件期间粒料的破坏。在震荡测试之后样品再次在0.5mm下的筛分测试2分钟以测定粒料的破坏程度。高温震荡测试在空气和氮气气氛中进行。碾磨熔渣细粒(样品SF1)的造粒测试结果见表2。这些结果显示大约2-4％的粘结剂加入得到关于粒料冷强度和高温震荡测试的最好结果。
表2
Figure C20058000996300091
％是质量％
除这些测试以外，对碾磨熔渣的不同尺寸级分(样品SF1，SF2和SF 3)进行相似的测试。采用粘结剂加粒量2.56质量％进行这些测试。这些测试的结果见表3。这些结果显示优选是熔渣的碾磨以获得具有足够高温强度的粒料。
表3
Figure C20058000996300101
％是质量％
采用此方式生产的粒料的碳含量典型地为约1质量％。这导致大约85的计算的(TiO2和FeO)/C质量比。
实施例2
将二氧化钛熔渣细粒(d50为125μm)碾磨到17μm的d50(来自实施例1的样品SF1)。然后使用胶凝化玉米淀粉作为粘结剂(粘结剂加料量为2.56质量％)，在盘式造粒机中附聚这些碾磨的细粒。在附聚工艺期间加入足够的水以协助附聚工艺。在附聚之后，将产物在60℃下干燥过夜。干燥的附聚产物的-850+106μm尺寸级分然后用于氯化测试工作。附聚产物的堆积密度为1.41g/cm3和(TiO2和FeO)/C质量比再次是大约85。在干燥之后附聚产物的组成如下(表4)：
表4
  SiO<sub>2</sub>(％)   Al<sub>2</sub>O<sub>3</sub>(％)   Fe<sub>总</sub>(％)   TiO<sub>2</sub>(％)   CaO(％)   MgO(％)   MnO(％)   Cr<sub>2</sub>O<sub>3</sub>(％)   V<sub>2</sub>O<sub>5</sub>(％)   C(％)
  2.45   1.20   8.45   82.5   0.17   0.94   1.88   0.15   0.37   1.12
％是质量％
附聚产物的氯化在外部加热的流化床反应器(内径50mm)中进行。氮气(6.5升每分钟)用于流化附聚样品(20g)同时将反应器加热到1000℃。当温度达到1000℃时，除氮气以外将CO(2.8升每分钟)和Cl2(4.0升每分钟)气体引入反应器。将产物气体在水冷却的冷凝器中冷却。在氢氧化钠溶液中吸收氯化物产物和过量氯气。允许反应持续15分钟，其后CO和Cl2气体流中断和切断炉动力。将流化床反应器用氮气冲洗5分钟，其后从反应器脱除残余物。残余物组成如下(表5)：
表5
  SiO<sub>2</sub>(％)   Al<sub>2</sub>O<sub>3</sub>(％)   Fe<sub>总</sub>(％)   TiO<sub>2</sub>(％)   CaO(％)   MgO(％)   MnO(％)   Cr<sub>2</sub>O<sub>3</sub>(％)   V<sub>2</sub>O<sub>5</sub>(％)   C(％)
  3.13   1.02   0.11   95.3   0.19   0.24   0.06   0.04   0.02   0.004
％是质量％
残余物的检查揭示附聚粒子的颜色从黑色变成米色。也注意到附聚粒子保持它们的整体性和不破裂成细粒，指示作为氯化原料的附聚产物的稳定性。
实施例3
将衍生自海滩沙钛铁矿的高二氧化钛熔渣细粒(分析相似于实施例1，表1；80质量％熔渣-75μm)使用各种类型有机粘结剂经历造粒测试。使用如下粘结剂：
●胶凝化玉米淀粉
●Peridur(羧甲基纤维素产品)(Peridur是商品名和它由AksoNobel提供)。
在每种情况下将熔渣细粒(2.5kg)与粘结剂在高强度混合机中在造粒步骤之前混合。盘式造粒机用于材料的造粒。将生产的微粒料在60℃下干燥过夜。从每个测试，-1+0.5mm级分(500g)筛分出。然后将此样品在轨道震动器上筛分4分钟和确定-0.5mm材料的数量。这用作粒料冷强度的定量测量。这些测试的结果见表6。
表6
  粘结剂   粘结剂加料(％)   冷强度：在-0.5mm下筛分的空气干燥粒料
  淀粉   2.00   1.56
  Peridur   1.00   1.54
注意到淀粉以及Peridur得到对粒料的粘结性能(相似的冷强度数值)。如果与其中Peridur用作粘结剂的粒料相比，采用淀粉作为粘结剂在球形成期间的物理粘结更容易。
实施例4
此实施例说明附聚的二氧化钛熔渣(粒料)与碾磨到-850+106μm尺寸级分的熔渣(氯化物等级熔渣)的氯化行为。
将衍生自海滩沙钛铁矿的二氧化钛熔渣细粒(d50为125μm)碾磨到20μm的d50。然后使用胶凝化玉米淀粉作为粘结剂(粘结剂加料量为2.56质量％)，在盘式造粒机中附聚这些碾磨的细粒。在附聚工艺期间加入足够的水以协助附聚工艺。在附聚之后，将产物在60℃下干燥过夜。干燥的附聚产物的-1+0.5mm尺寸级分然后用于氯化测试工作。附聚产物的d50测量为690μm，同时产物的堆积密度为1.47g/cm3。(TiO2和FeO)/C质量比是114。在干燥之后附聚产物的组成如下(表7)：
表7
  SiO<sub>2</sub>(％)   Al<sub>2</sub>O<sub>3</sub>(％)   Fe<sub>总</sub>(％)   TiO<sub>2</sub>(％)   CaO(％)   MgO(％)   MnO(％)   Cr<sub>2</sub>O<sub>3</sub>(％)   V<sub>2</sub>O<sub>5</sub>(％)   C(％)
  2.54   1.21   8.3   81.4   0.12   0.94   1.79   0.22   0.44   0.81
％是质量％
将二氧化钛熔渣碾磨到-850+106μm尺寸级分。此样品的d50测量为370μm，及堆积密度为2.03g/cm3。此样品的组成如下(表8)：
表8
  SiO<sub>2</sub>(％)   Al<sub>2</sub>O<sub>3</sub>(％)   Fe<sub>总</sub>(％)   TiO<sub>2</sub>(％)   CaO(％)   MgO(％)   MnO(％)   Cr<sub>2</sub>O<sub>3</sub>(％)   V<sub>2</sub>O<sub>5</sub>(％)   C(％)
  2.12   1.26   7.5   85.2   0.12   0.97   1.75   0.22   0.46   0.03
％是质量％
这些产物的氯化在石英管(27mm直径)中进行。多孔玻璃料负载由如下物质组成的样品床层：一种熔渣样品以及含碳还原剂(Sascarb LS)的混合物。通过将装料(40g熔渣样品和8g Sascarb LS)放入反应器进行测试。将氮气通过反应器，在此期间它达到1200℃的温度。当床层达到1200℃时除氮气以外引入氯气。在测试完成之后在氮气中冷却床层。
熔渣粒料和氯化物等级熔渣的对比氯化结果见表9。表9显示从反应器床脱除的FeO和TiO2级分。FeO氯化快速，而TiO2在样品中的氯化较缓慢。这些结果显示在两种样品之间的氯化速率相似。
表9
Figure C20058000996300131
也测量在氯化之后在床层中剩余的熔渣的d50。对于熔渣粒料，在所有测试的氯化之后的d50为400-700μm，指示在氯化工艺期间发生的最小粒料破裂。对于氯化物等级熔渣，在氯化之后的典型d50是300-400μm，指示氯化物等级熔渣的最小破裂。
从这些结果得出的结论是熔渣粒料可以用作氯化物等级熔渣的替代物。

Claims (19)

1.一种二氧化钛熔渣粒子的附聚方法，包括：
-提供d50粒度小于106μm的二氧化钛熔渣；
-混合熔渣粒子与有机粘结剂；和
-使熔渣粒子和有机粘结剂的混合物附聚成d50粒度为106μm-1000μm的附聚粒子和附聚粒子的(TiO2和FeO)/C质量比大于3.4。
2.权利要求1的方法，其中二氧化钛熔渣的TiO2含量按质量计大于75％。
3.权利要求1或2的方法，其中熔渣是衍生自海滩沙钛铁矿的熔渣。
4.权利要求1的方法，包括调整二氧化钛熔渣大小到d50粒度小于106μm的步骤。
5.权利要求4的方法，其中通过碾磨来调整大小。
6.权利要求1的方法，其中熔渣的d50粒度小于40μm。
7.权利要求1的方法，其中有机粘结剂选自纤维素产物、乳品场废产物、天然树胶、淀粉产物、淀粉丙烯酸类共聚物、半纤维素产物中的一种或多种的混合物。
8.权利要求7的方法，其中粘结剂是胶凝化玉米淀粉。
9.权利要求8的方法，其中混合二氧化钛熔渣和胶凝化玉米淀粉以包含按质量计1-5％胶凝化玉米淀粉。
10.权利要求1的方法，其中通过造粒使调整过大小的熔渣和粘结剂的混合物附聚。
11.权利要求1的方法，其中附聚粒子的d50粒度为150-1000μm。
12.权利要求1的方法，其中(TiO2和FeO)/C质量比大于4。
13.权利要求12的方法，其中(TiO2和FeO)/C质量比为至少20。
14.权利要求13的方法，其中(TiO2和FeO)/C质量比大于40。
15.权利要求1的方法，其中将形成的附聚粒子经历热处理。
16.一种附聚的二氧化钛熔渣粒子，含有d50粒度为106-1000μm的附聚粒子，和附聚粒子的(TiO2和FeO)/C质量比大于3.4。
17.从二氧化钛熔渣生产TiO2的氯化物方法，其中使用由权利要求1-15任意一项的方法制备的附聚的二氧化钛熔渣粒子。
18.从二氧化钛熔渣生产TiO2的氯化物方法，其中使用权利要求16的附聚的二氧化钛熔渣粒子。
19.权利要求17或18任一项的从二氧化钛熔渣生产TiO2的氯化物方法，包括如下步骤：
-提供附聚的二氧化钛熔渣粒子；
-供应附聚的二氧化钛熔渣与还原剂和氯气到流化床反应器中以生产气态四氯化钛；
-冷凝气态四氯化钛；和
-氧化冷凝的四氯化钛以形成TiO2。
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CN102776365A (zh) * 2012-06-12 2012-11-14 攀钢集团攀枝花钢铁研究院有限公司 一种细粒级钛原料的团粒方法
WO2016005041A1 (de) * 2014-07-08 2016-01-14 Kronos International, Inc. Verfahren zur agglomeration feinteiliger rohstoffe für die titandioxidherstellung
JP7008639B2 (ja) * 2016-05-19 2022-01-25 イルカ・リソーシズ・リミテッド チタン含有材料の細粒の凝集
CN110563034B (zh) * 2019-09-29 2022-05-17 河南佰利联新材料有限公司 一种使用富钛细粉料制备氯化法TiO2原料的方法
CN110627119B (zh) * 2019-09-29 2022-05-13 河南佰利联新材料有限公司 一种使用含钛细粉料制备氯化法TiO2原料的方法
CN113634357B (zh) * 2021-08-23 2024-02-13 云南国钛金属股份有限公司 一种四氯化钛收尘渣的回收方法
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