CN1347345A - 用于铁矿石中硅酸盐的泡沫浮选的季铵化合物 - Google Patents
用于铁矿石中硅酸盐的泡沫浮选的季铵化合物 Download PDFInfo
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Abstract
本发明涉及一种泡沫浮选法,其中在含季铵化合物的浮选促集剂存在的情况下,将硅酸盐从铁矿石中分离出来,其中季铵化合物的分子式为R1R1N+R3R41/z Xz－(I),其中R1独立为烃基,优选为含6－14个碳原子的脂族基和/或R2－(OR7)m－OR8－,其中R2独立为含6－14个碳原子的酰基,R7独立为含2－4个碳原子的亚烷基,R8独立为含2－3个碳原子的亚烷基,m为0－5的数字,R3和R4独立为含1－4个碳原子的烷基或(R5O)P,其中R5独立为含2－4个碳原子的亚烷基,p为1－4的数字,X为负离子基团,且z为负离子X的电荷数。该浮选促集剂对于富集泡沫产品中的硅酸盐有很高的选择性,同时在底部富集体中保持了很高的铁矿石产率。
Description
本发明涉及一种泡沫浮选法，其中在含有带两个脂族基和/或带含有6-14个碳原子的酰基的季铵化合物的浮选促集剂存在下，将硅酸盐从铁矿石中分离出来。这种浮选促集剂对于富集泡沫产品中的硅酸盐有很高的选择性，同时在底部富集体或富集体中保持了很高的铁矿石产率。
在泡沫浮选中常常使用季铵化合物作为浮选促集剂。因此，在WO94/26419中已公开了在含季铵化合物和烷基胺的烯化氧加合物作为浮选促集剂组分的混合物存在的情况下，用泡沫浮选法处理方解石矿。WO97/26995中描述了四酯(esterquat)作为非硫化(nonsulphidic)矿物的浮选促集剂的用途。季铵化合物含有6-24个碳原子的酰基。在操作实例中，用没有限定特征的四酯、二椰油烷基二甲基氯化铵或三甲基牛油烷基氯化铵作为高镁含量的富硅酸盐方解石矿的浮选促集剂。US 3 960 715涉及在包括季胺，例如十二烷基三甲基氯化铵在内的阳离子浮选促集剂存在的情况下从铁矿石中分离出硅脉石组分的泡沫浮选法。
文章“Cationic Flotation of Silica From Magnetic Iron-oreConcentrates”：H.C.Hedberg，MAOCS，U7(1970：5，177-179)中，比较了不同阳离子浮选促集剂的影响。测试表明，季铵化合物、三甲基椰油烷基氯化铵、三甲基月桂基氯化铵和三甲基牛油烷基氯化铵没有用作标准的乙酸椰油烷基伯胺有效。
美国专利US 4 995 998公开了在非硫化矿浮选中用憎水基团封端的脂肪醇聚乙二醇醚与阳离子或两性表面活性剂一起作为共浮选促集剂的用途。其实施例4中，在月桂基三甲基氯化铵存在的情况下将纯石英砂用于泡沫浮选法。
尽管这种浮选法有积极的影响，但也存在一个明显的趋势，即富集的铁矿石中硅酸盐水平太高(常超过1重量％)或铁产率太低。因此，本发明的主要目的是开发一种硅酸盐含量低且铁含量高的选择性更好的泡沫浮选法。
根据本发明，已发现在铁矿石沉淀剂和季铵化合物存在的情况下，且含硅酸盐铁矿石水悬浮液的pH值为7-11的条件下进行反向泡沫浮选可达到该目的，该季铵化合物的分子式为
R1R1N+R3R4 1/z Xz- (I)，其中R1独立为烃基，优选为含6-14个碳原子的脂族基和/或R2-(OR7)m-OR8-，其中R2独立为含6-14个碳原子的酰基，R7独立为含2-4个碳原子的亚烷基，R8独立为含2-3个碳原子的亚烷基，m为0-5的数字，R3和R4独立为含1-4个碳原子的烷基或(R5O)p，其中R5独立为含2-4个碳原子的亚烷基，p为1-4的数字，X为负离子基团，且z为负离子X的电荷数，每千克铁矿石需季铵化合物的量为10-500毫克。
优选R1为含6-10个碳原子的直链脂族基或含8-13个碳原子的支链脂族基，且R2为含6-10个碳原子的直链酰基或含8-13个碳原子的支链酰基。
这种带有两个相对小的脂族基和/或酰基的季铵化合物，即使以很低的剂量也会表现出意想不到的高的硅酸盐选择性，并且得到高纯度的含铁富集体和非常低的硅酸盐含量。优选每千克铁矿石加入15-200毫克的季铵化合物，最优选每千克铁矿石加入15-100毫克。
因为由粗浮选所得的泡沫产品可含有大量的铁矿石，在加水以后，且如果需要，另外再加入季铵化合物、沉淀剂和/或其它浮选化学制剂以后，可以对泡沫产品进行一次或多次的泡沫浮选(清洗步骤)，例如1到5次。通常，没有必要再补充加入任何浮选促集剂。将由粗浮选所得的底部富集体和由泡沫产品进行随后泡沫浮选所得的底部富集体适当混合为铁产率高且硅酸盐含量低的最终富集体。
优选季铵化合物为那些，其中R5、R7和R8为-C2H4-，且至少R3和R4之一为烷基，优选为甲基。这些化合物易于生产且性能很好。R1优选为正辛基、正癸基、2-丙基庚基和/或含9-13个碳原子的甲基取代的烷基。R2优选为2-乙基己酰基、正辛酰基、2-丙基庚酰基和含9-13个碳原子的甲基取代的酰基。阴离子X适宜地为卤化物，例如氯化物；烷基硫酸盐，例如甲基硫酸盐；硫酸；或羧酸盐，例如乙酸盐。浮选法中所用的季铵化合物已熟知，并且有公开其制备方法的文献综述.
根据本发明的所述的浮选法，可以将铁矿石与水一起碾碎为所需的尺寸。原则上，至少50重量％的矿粉颗粒尺寸在5到200μm之间。然后将矿粉悬浮在水中，并用通常的方法，例如过筛、沉淀或离心分离等方法将细料脱矿泥。然后，由细料矿石制备水浆(浆)，并且正常加入铁矿石沉淀剂。沉淀剂可以是亲水的多糖，例如淀粉，例如用碱和糊精活化处理的玉米淀粉。其它的合适的亲水多糖实例是纤维素衍生物，例如羧甲基纤维素，磺甲基纤维素，甲基纤维素，羟乙基纤维素和乙基羟乙基纤维素；亲水树胶，例如阿拉伯树胶，刺梧桐树胶，黄蓍树胶，印度胶；藻酸盐；和淀粉衍生物，例如羧甲基淀粉和磷酸盐淀粉。沉淀剂正常的加入量为每吨矿石约10到约1000克。此外，碱的加入量通常足以使pH值达到7-11，优选地为9-11。将浆料准备好以后，可加入季铵化合物，并且在进行泡沫浮选以前将混合物进一步稳定一会儿。如果需要，在泡沫浮选以前可以在方便的时候加入泡沫调节剂。适当的泡沫调节添加剂的实例为甲基异丁基甲醇和任选地用环氧乙烷和/或环氧丙烷烷氧基化的带有6-12个碳原子的醇。
下面进一步通过实施例解释本发明。
实施例1
将含有约13.1重量％的SiO2和约85.9重量％的Fe2O3的赤铁矿碾碎到可以使45.4重量％通过32μm的网眼的筛子的颗粒尺寸。然后将矿石悬浮在水中，并用旋液分离器脱泥浆，脱泥浆矿石的水浆制备成干含量为60％。每千克矿石添加500mL用碱处理的淀粉后，将浆料稳定5分钟。将浆料中矿石的浓度加水稀释到40％，将浆料的pH值调到10.5，并按表2中所述的量加入浮选促集剂。将整个混合物稳定60秒，接着进行粗浮选，由此获得富硅酸盐泡沫产品和富铁底部富集体。不加任何浮选促集剂或其它添加剂通过二次浮选(清洗步骤)清洗泡沫产品，并将清洗所得的底部富集体加到粗浮选所得的底部富集体中。重复一或三次该清洗步骤，并将不同清洗步骤所得的底部富集体混合。分析粗浮选所得的底部富集体和不同的混合底部富集体的铁(Fe2O3)产率和硅酸盐(SiO2)含量。其结果列示在下表2中。
表1浮选促集剂
表2浮选结果
从该结果可见，本发明所述的富集体有很强的硅酸盐选择性和亲和力。通过泡沫产品的重复清洗，与现有技术相比，本方法也可能获得优异的Fe2O3产率且SiO2含量非常低的底部富集体混合物。此外，该泡沫浮选法所需的浮选促集剂用量惊人地低。
| 编号 | 结构 |
| A | C8-C10-烷基-O-C3H6 NH2 |
| B | 椰油脂肪烷基(CH3)3N+Cl- |
| 1 | (正辛基)2(CH3)2N+Cl- |
| 2 | (2-乙基己基-OC2H4)2(CH3)2N+Cl- |
| 3 | 20％(正辛基)2(CH3)2N+Cl-80％(正癸基)2(CH3)2N+Cl- |
| 编号 | 加入量(mg/kg矿石) | 底部富集体 | |||||||||
| Fe2O3产率(％) | SiO2含量(％) | ||||||||||
| A | 30 | 90.8 | 98.0 | 99.7 | - | - | 0.79 | 2.02 | 4.85 | - | - |
| B | 60 | 69.0 | 81.1 | 87.6 | - | - | 1.11 | 2.65 | 4.85 | - | - |
| 1 | 20 | 81.4 | 91.3 | 94.2 | 96.7 | 98.2 | 0.59 | 0.68 | 0.77 | 0.88 | 1.12 |
| 1 | 25 | 75.0 | 87.9 | 92.8 | 95.3 | 97.3 | 0.49 | 0.53 | 0.55 | 0.59 | 0.69 |
| 2 | 30 | 78.4 | 89.5 | 93.9 | 96.0 | 97.7 | 0.59 | 0.62 | 0.66 | 0.71 | 0.82 |
| 3 | 45 | 79.4 | 90.6 | 94.9 | - | - | 0.54 | 0.66 | 0.80 | - | - |
实施例2
将含有24.1重量％的SiO2和约73.6重量％的Fe2O3的赤铁矿碾碎到可以使27.2重量％通过32μm的网眼的筛子的颗粒尺寸。然后按如实施例1同样的方法制备碾碎了的物料的水悬浮液。将铁矿石悬浮液进行粗浮选，随后进行一步或多步泡沫产品的清洗。在浮选过程中，没有额外加入浮选化学制剂。分析粗浮选所得的底部富集体和不同的混合底部富集体的铁(Fe2O3)产率和硅酸盐(SiO2)含量。其结果列示在下表4中。
表3浮选促集剂
表4浮选结果
| 编号 | 加入量(mg/kg矿石) | 底部富集体 | |||||||||
| Fe2O3产率(％) | SiO2含量(％) | ||||||||||
| A | 100 | 86.3 | 96.3 | 98.8 | - | - | 1.2 | 2.3 | 4.1 | - | - |
| B | 200 | 77.7 | 91.1 | - | - | - | 24.1 | 24.8 | - | - | - |
| C | 200 | 74.7 | 89.0 | - | - | - | 1.2 | 1.3 | - | - | - |
| C | 100 | 82.1 | 94.4 | - | - | - | 8.2 | 10.2 | - | - | - |
| 1 | 45 | 84.4 | 93.6 | 96.4 | 97.7 | 98.4 | 0.91 | 1.01 | 1.12 | 1.23 | 1.4 |
| 1 | 60 | 81.5 | 91.4 | 94.9 | - | - | 0.88 | 0.96 | 1.06 | - | - |
| 2 | 45 | 86.8 | 94.8 | 97.3 | - | - | 0.98 | 1.08 | 1.18 | - | - |
| 2 | 60 | 83.1 | 92.2 | 95.3 | - | - | 0.87 | 0.97 | 1.07 | - | - |
| 3 | 60 | 86.1 | 94.8 | - | - | - | 0.97 | 1.2 | - | - | - |
| 4 | 60 | 89.3 | 96.8 | - | - | - | 1.02 | 1.4 | - | - | - |
| 5 | 100 | 92.7 | 98.6 | - | - | - | 0.85 | 1.3 | - | - | - |
| 6 | 150 | 92.4 | 98.5 | - | - | - | 0.98 | 1.5 | - | - | - |
浮选结果与实施例1相似。本发明所述的浮选促集剂，特别是带有短的脂族基或酰基的浮选促集剂，加入很少的量就有很强的硅酸盐选择性和亲和力。
Claims (9)
1.一种从富硅酸盐铁矿中富集铁矿石的方法，其通过在含季铵化合物和铁矿石沉淀剂且pH值为7-11的条件下，对铁矿石水悬浮液反向泡沫浮选，其特征在于下式的浮选促集剂
R1R1N+R3R4 1/z Xz- (I)，
其中R1独立为烃基，优选为含6-14个碳原子的脂族基和/或R2-(OR7)m-OR8-，其中R2独立为含6-14个碳原子的酰基，R7独立为含2-4个碳原子的亚烷基，R8独立为含2-3个碳原子的亚烷基，m为0-5的数字，R3和R4独立为含1-4个碳原子的烷基或(R5O)p，其中R5独立为含2-4个碳原子的亚烷基，p为1-4的数字，X为负离子基团，且z为负离子X的电荷数，每千克铁矿石需季铵化合物的量为10-500毫克。
2.根据权利要求1所述的方法，其特征在于，R1独立为含6-10个碳原子的直链脂族基或含8-13个碳原子的支链脂族基或R2-(OR7)m-OR8-，其中R7，R8，m的含意同权利要求1，并且R2独立为含6-10个碳原子的直链酰基或含8-13个碳原子的支链酰基。
3.根据权利要求1或2所述的方法，其特征在于，R5、R7和R8为-C2H4-，且至少R3和R4之一为烷基。
4.根据权利要求1、2或3所述的方法，其特征在于，每千克铁矿石需季铵化合物15-200毫克。
5.根据权利要求1-4任一项所述的方法，其特征在于，R1独立为正辛基、正癸基、2-丙基庚基和/或含9-13个碳原子的甲基取代的烷基。
6.根据权利要求1-4任一项所述的方法，其特征在于，R2独立为2-乙基己酰基、正辛酰基、2-丙基庚酰基和含9-13个碳原子的甲基取代的酰基。
7.根据权利要求1-6任一项所述的方法，其特征在于，在加入季铵化合物之前，将亲水多糖作为铁矿石沉淀剂加入到水悬浮液中。
8.根据权利要求7所述的方法，其特征在于，将由铁矿石的水悬浮液浮选所得的泡沫产品至少进行一次额外泡沫浮选。
9.如权利要求1-6所定义的季铵化合物用作浮选促集剂的用途，该浮选促集剂用于通过反向泡沫浮选法从富硅酸盐铁矿石中富集铁矿石。
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| SE9901398A SE514435C2 (sv) | 1999-04-20 | 1999-04-20 | Kvartära ammoniumföreningar för skumflotation av silikater från järnmalm |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101337204B (zh) * | 2008-08-13 | 2011-03-30 | 中南大学 | 一种双季铵盐类化合物在硅酸盐矿物浮选上的应用及硅酸盐矿物浮选捕收剂 |
| CN102112235A (zh) * | 2008-11-07 | 2011-06-29 | 科莱恩金融(Bvi)有限公司 | 作为用于含硅酸盐矿物的捕收剂的由胺烷氧基化酯和季铵化合物组成的混合物 |
| CN102933310A (zh) * | 2010-05-28 | 2013-02-13 | 阿克佐诺贝尔化学国际公司 | 季铵化合物在泡沫浮选法中作为促集剂的用途 |
| CN104822460A (zh) * | 2012-10-01 | 2015-08-05 | 凯米罗总公司 | 矿物矿石浮选的抑制剂 |
| CN105396698A (zh) * | 2015-11-19 | 2016-03-16 | 中钢集团马鞍山矿山研究院有限公司 | 一种复合型季铵盐阳离子硅酸盐矿物捕收剂及其制备方法 |
| CN106733209A (zh) * | 2015-11-19 | 2017-05-31 | 中钢集团马鞍山矿山研究院有限公司 | 一种微细粒铁矿石反浮选捕收剂的制备方法 |
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| DE102006010939A1 (de) | 2006-03-09 | 2007-09-13 | Clariant International Limited | Flotationsreagenz für Silikate |
| DE102006019561A1 (de) | 2006-04-27 | 2007-10-31 | Clariant International Limited | Flotationsreagenz für silikathaltige Mineralien |
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| DE102010004893A1 (de) | 2010-01-19 | 2011-07-21 | Clariant International Limited | Flotationsreagenz für magnetit- und/oder hämatithaltige Eisenerze |
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| CN102941160A (zh) * | 2012-12-13 | 2013-02-27 | 贵州大学 | 一种硅酸盐矿物浮选捕收剂 |
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| US4830739A (en) * | 1985-02-20 | 1989-05-16 | Berol Kemi Ab | Process and composition for the froth flotation beneficiation of iron minerals from iron ores |
| DE3818482A1 (de) | 1988-05-31 | 1989-12-07 | Henkel Kgaa | Tensidmischungen als sammler fuer die flotation nichtsulfidischer erze |
| US4892649A (en) * | 1988-06-13 | 1990-01-09 | Akzo America Inc. | Calcium carbonate beneficiation |
| SE501623C2 (sv) | 1993-05-19 | 1995-04-03 | Berol Nobel Ab | Sätt att flotera kalciumkarbonatmalm samt ett flotationsreagens därför |
| DE19602856A1 (de) | 1996-01-26 | 1997-07-31 | Henkel Kgaa | Biologisch abbaubare Esterquats als Flotationshilfsmittel |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101337204B (zh) * | 2008-08-13 | 2011-03-30 | 中南大学 | 一种双季铵盐类化合物在硅酸盐矿物浮选上的应用及硅酸盐矿物浮选捕收剂 |
| CN102112235A (zh) * | 2008-11-07 | 2011-06-29 | 科莱恩金融(Bvi)有限公司 | 作为用于含硅酸盐矿物的捕收剂的由胺烷氧基化酯和季铵化合物组成的混合物 |
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| CN102933310B (zh) * | 2010-05-28 | 2014-04-16 | 阿克佐诺贝尔化学国际公司 | 季铵化合物在泡沫浮选法中作为促集剂的用途 |
| CN104822460A (zh) * | 2012-10-01 | 2015-08-05 | 凯米罗总公司 | 矿物矿石浮选的抑制剂 |
| CN105396698A (zh) * | 2015-11-19 | 2016-03-16 | 中钢集团马鞍山矿山研究院有限公司 | 一种复合型季铵盐阳离子硅酸盐矿物捕收剂及其制备方法 |
| CN106733209A (zh) * | 2015-11-19 | 2017-05-31 | 中钢集团马鞍山矿山研究院有限公司 | 一种微细粒铁矿石反浮选捕收剂的制备方法 |
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| ZA200108190B (en) | 2003-04-30 |
| EA003556B1 (ru) | 2003-06-26 |
| AU763599B2 (en) | 2003-07-24 |
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| BR0000157A (pt) | 2001-01-16 |
| CA2366948A1 (en) | 2000-10-26 |
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| NO20014978L (no) | 2001-10-12 |
| AU4631600A (en) | 2000-11-02 |
| WO2000062937A1 (en) | 2000-10-26 |
| SE9901398D0 (sv) | 1999-04-20 |
| BR0000157B1 (pt) | 2011-05-17 |
| OA11860A (en) | 2006-03-02 |
| SE514435C2 (sv) | 2001-02-26 |
| US7311206B1 (en) | 2007-12-25 |
| UA71956C2 (uk) | 2005-01-17 |
| EG22704A (en) | 2003-07-30 |
| SE9901398L (sv) | 2000-10-21 |
| NO20014978D0 (no) | 2001-10-12 |
| CN1130269C (zh) | 2003-12-10 |
| NO321799B1 (no) | 2006-07-03 |
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