CN107107075A - 用于非硫化物矿物的改进的浮选的脂肪酸和肌氨酸的n‑酰基衍生物的组合物 - Google Patents
用于非硫化物矿物的改进的浮选的脂肪酸和肌氨酸的n‑酰基衍生物的组合物 Download PDFInfo
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Abstract
本发明涉及用于非硫化物矿石的直接泡沫浮选的捕集剂组合物,其包含a)50‑99重量%的脂肪酸的混合物和b)1‑50重量%的式(I)的肌氨酸的N‑酰基衍生物,其中R为具有7‑21个碳原子的饱和或不饱和烃链,其中所述混合物包含10.0‑35.0重量%的具有饱和C11烃基的脂肪酸、2.5‑15.0重量%的具有饱和C13烃基的脂肪酸、10.0‑25.0重量%的具有单不饱和C17烃基的脂肪酸肪酸和20.0‑45.0重量%的具有双不饱和C17烃基的脂肪酸。
Description
本发明涉及包含至少两种脂肪酸和至少一种肌氨酸的N-酰基衍生物的混合物的新的捕集剂组合物以及其在非硫化物矿物的直接泡沫浮选中的用途。使用所述新的捕集剂组合物提供了改进的浮选效率。
泡沫浮选是一种用于将被认为具有经济价值的矿物颗粒与认为是废物的那些分开的物理化学过程。它是基于空气气泡选择性地附着到先前被赋予疏水性的那些颗粒上的能力。然后,颗粒-气泡组合上升到泡沫相,从那里将其排出浮选槽,同时亲水性颗粒保留在浮选槽中。颗粒疏水性进而由称为捕集剂的特殊化学品引起。在直接浮选系统中,其为通过捕集剂的作用变得疏水的经济上有价值的矿物。类似地,在反向浮选系统中,捕集剂对被认为是废物的那些矿物颗粒赋予疏水性。分离过程的效率在回收率和品位方面进行量化。回收率是指在浮选后移入精矿流中的矿石中含有的有价值产品的百分比。品位是指浮选后精矿中具有经济价值的产品的百分比。回收率或品位的更高的值表示更有效的浮选系统。
使用脂肪酸和肌氨酸衍生物的混合物用于非硫化物矿物的泡沫浮选是众所周知的。
在DD-300730中,描述了使用包含肌氨酸的N-酰基衍生物和具有14-24个碳原子的烃链的饱和或不饱和脂肪酸的捕集剂组合物用于氟石的泡沫浮选。
在US-5147528中描述了直接浮选磷酸盐的方法,其中将含有12-36个碳原子的脂肪酸、妥尔油沥青、衍生自植物的胺、肌氨酸和燃料油或炉油的氧化的均质混合物用作捕集剂。
US-4514290描述了一种捕集剂组合物,其包含脂肪酸或其盐,含有有机疏水基团的酰氨基羧酸或酰氨基磺酸或其盐,以及磷酸和至少一种烷氧基化醇的偏酯。据称这样的组合物显示出对于含有碱土金属的矿物如磷灰石、白钨矿、菱镁矿和重晶石的泡沫浮选具有改进的效率。优选的组合物中的脂肪酸具有14-22个碳原子。
WO-2014040686描述了磷酸盐矿石的浮选剂,其包含至少一种脂肪酸和至少一种肌氨酸的N-酰基衍生物。
本发明涉及包含至少两种脂肪酸和至少一种肌氨酸的N-酰基衍生物的混合物的新的捕集剂组合物及其用于非硫化物矿物的选矿的用途。根据本发明的至少两种脂肪酸和至少一种N-酰基衍生物的组合物与通过现有技术描述的捕集剂组合物相比提供浮选效率的改进。改进的浮选效率意味着实现更高的矿物回收率和/或纯度。此外,根据本发明的捕集剂组合物非常容易通过简单混合制备,并且不需要任何额外的处理,例如氧化步骤,从而显示出浮选效率的极好的改进。
不可预料地发现,含有50-99重量%的至少两种脂肪酸的混合物和1-50重量%的肌氨酸的N-酰基衍生物的组合物在更高的矿物回收率和/或更高的纯度方面显示出非硫化物矿物的改进的浮选。
因此,本发明涉及捕集剂组合物,其包含
a)50-99重量%的脂肪酸的混合物,和
b)1-50重量%的式(I)的肌氨酸的N-酰基衍生物
其中
R为具有7-21个碳原子的饱和或不饱和烃链,其中脂肪酸的混合物包含10.0-35.0重量%的具有饱和C11烃基的脂肪酸、2.5-15.0重量%的具有饱和C13烃基的脂肪酸、10.0-25.0重量%的具有单不饱和C17烃基的脂肪酸和20.0-45.0重量%的具有双不饱和C17烃基的脂肪酸。
本发明的捕集剂组合物可以包含达到100重量%的余量的其它脂肪酸。重量百分数是指作为100重量%的本发明的捕集剂组合物的总脂肪酸含量。
在优选实施方案中,脂肪酸的混合物包含具有以下的脂肪酸
1.0-6.5重量%的饱和C7
1.0-4.0重量%的饱和C9
10.0-35.0重量%的饱和C11
2.5-15.0重量%的饱和C13
1.0-7.0重量%的饱和C15
0.0-1.0重量%的单不饱和C15
0.0-1.0重量%的双不饱和C15
0.5-2.0重量%的饱和C17
10.0-25.0重量%的单不饱和C17
20.0-45.0重量%的双不饱和C17
0.0-2.0重量%的三不饱和C17
0.0-1.0重量%的饱和C19
0.0-4.0重量%的单不饱和C19烃链,和
0.0-7.0重量%的其它脂肪酸。
表述“饱和烃链”优选是指烷基。表述“单饱和烃链”优选是指烯基。表述“双不饱和烃链”是指具有两个双键的烯基。
脂肪酸在本发明的意义上被定义为带有长直链烃链的羧酸的混合物,所述羧酸可以是饱和的或不饱和的或多不饱和的。对本发明的范围特别有效的是使用来自植物油的脂肪酸和妥尔油脂肪酸。在本发明的意义上优选的脂肪酸是椰子油脂肪酸和妥尔油脂肪酸。椰子油脂肪酸中的主要羧酸是含量为44-54重量%的月桂酸(饱和C11烃链)和含量为13-20重量%的肉豆蔻酸(饱和C13烃链)。优选品质的妥尔油脂肪酸的酸值高于190mg KOH/g,松香酸和不可皂化物的含量分别低于2.1重量%和2.0重量%。妥尔油脂肪酸中的主要羧酸是含量为25-50重量%的油酸(单不饱和C17烃链)和含量为35-60重量%的亚油酸(双不饱和C17烃链)。
脂肪酸中烷基链分布的表征可以通过气相色谱法在挥发性甲酯衍生物中的羧酸转化后根据AOCS方法Ce 1-62,“Fatty Acid Composition by Gas Chromatography”,AOCSOfficial Methods(2005)American Oil Chemists Society进行。
在根据本发明的捕集剂组合物中特别有效的脂肪酸混合物含有0.3-1.7重量份的来自植物油的脂肪酸比1重量份的妥尔油脂肪酸。根据本发明的脂肪酸的混合物的最优选的比例是1重量份的椰子油脂肪酸比1重量份的妥尔油脂肪酸。
特别优选的是肌氨酸的N-酰基衍生物,其中R是具有11-19个碳原子的饱和或不饱和烃链。最优选的肌氨酸的N-酰基衍生物是N-油酰基肌氨酸。
根据本发明的特别优选的捕集剂组合物含有65-99重量%的脂肪酸的混合物(组分a)和1-35重量%的肌氨酸的N-酰基衍生物(组分b)。最优选的捕集剂组合物含有80重量%的椰子油脂肪酸和妥尔油脂肪酸的1:1重量的混合物和20重量%的N-油酰基肌氨酸。
本发明的组合物用作非硫化物矿石的直接泡沫浮选方法中的捕集剂。已发现本发明的组合物特别适合用于含有碱土金属的非硫化物矿石,如磷灰石、方解石、白钨矿、萤石、菱镁矿和重晶石的直接泡沫浮选。最令人惊奇地发现,本发明的组合物还特别适合用于钛铁矿的直接泡沫浮选,钛铁矿是钛的最重要来源的式FeTiO3的钛铁氧化物矿物。
此外,本发明还涉及非硫化物矿物的选矿方法,该方法包括使根据本发明的捕集剂组合物与非硫化物矿物的含水悬浮液接触并使如此形成的矿浆起泡沫的步骤。根据本发明的捕集剂组合物优选以100-1000g/t固体矿石的量用于非硫化物矿石的直接泡沫浮选。如果需要,还可以向矿浆中加入其它浮选试剂。这些试剂的实例是起泡剂,例如松油,聚二醇,聚氧化石蜡(polyoxyparaffin)或醇,抑制剂,例如淀粉,羧甲基纤维素或硅酸钠,和pH调节剂,例如氢氧化钠或碳酸钠。
实施例
1.制备根据本发明的捕集剂组合物的一般程序:
将蒸馏的椰子脂肪酸样品温热至35℃,直到其完全熔化,然后在室温下添加至妥尔油脂肪酸。然后通过缓慢搅拌作用将脂肪酸混合物均质化。最后,将N-油酰基肌氨酸缓慢添加至脂肪酸混合物。然后将混合物均质化另外10分钟。当获得澄清的黄色液体溶液时,程序完成。
2.按照已使用的1所描述的程序如下制备根据本发明制备的收集剂组合物。
组合物1:
组分a:
80重量%的1重量份的蒸馏的椰子脂肪酸和1重量份的妥尔油脂肪酸的混合物,其具有如下的烃链分布:
3.25重量%的饱和C7烃链
2.85重量%的饱和C9
25.65重量%的饱和C11
8.60重量%的饱和C13
4.45重量%的饱和C15
0.02重量%的单不饱和C15
0.20重量%的双不饱和C15
1.25重量%的饱和C17
19.10重量%的单不饱和C17
28.5重量%的双不饱和C17
0.60重量%的三不饱和C17
0.05重量%的饱和C19
1.25重量%的单不饱和C19
4.3重量%的其它
组分b:
20重量%的N-油酰基肌氨酸
组合物2:
组分a:
80重量%的0.33重量份的蒸馏的椰子脂肪酸和1重量份的妥尔油脂肪酸的混合物,其具有如下的烃链分布:
1.62重量%的饱和C7烃链
1.42重量%的饱和C9
12.82重量%的饱和C11
4.30重量%的饱和C13
2.37重量%的饱和C15
0.04重量%的单不饱和C15
0.30重量%的双不饱和C15
1.17重量%的饱和C17
24.70重量%的单不饱和C17
42.15重量%的双不饱和C17
0.90重量%的三不饱和C17
0.02重量%的饱和C19
1.87重量%的单不饱和C19
6.40重量%的其它
组分b:
20重量%的N-油酰基肌氨酸
组合物3:
组分a:
80重量%的1.66重量份的蒸馏的椰子脂肪酸和1重量份的妥尔油脂肪酸的混合物,其具有如下的烃链分布:
4.10重量%的饱和C7烃链
3.59重量%的饱和C9
32.32重量%的饱和C11
10.84重量%的饱和C13
5.53重量%的饱和C15
0.02重量%的单不饱和C15
0.15重量%的双不饱和C15
1.29重量%的饱和C17
16.19重量%的单不饱和C17
21.40重量%的双不饱和C17
0.44重量%的三不饱和C17
0.06重量%的饱和C19
0.92重量%的单不饱和C19
3.21重量%的其它
组分b:
20重量%的N-油酰基肌氨酸
组合物4:
组分a:
67重量%的1重量份的蒸馏的椰子脂肪酸和1重量份的妥尔油脂肪酸的混合物,具有如下的烃链分布:
3.25重量%的饱和C7烃链
2.85重量%的饱和C9
25.65重量%的饱和C11
8.60重量%的饱和C13
4.45重量%的饱和C15
0.02重量%的单不饱和C15
0.20重量%的双不饱和C15
1.25重量%的饱和C17
19.10重量%的单不饱和C17
28.5重量%的双不饱和C17
0.60重量%的三不饱和C17
0.05重量%的饱和C19
1.25重量%的单不饱和C19
4.3重量%的其它
组分b:
33重量%的N-油酰基肌氨酸
组合物5:
组分a:
75重量%的1重量份的蒸馏的椰子脂肪酸和1重量份的妥尔油脂肪酸的混合物,其具有如下的烃链分布:
3.25重量%的饱和C7烃链
2.85重量%的饱和C9
25.65重量%的饱和C11
8.60重量%的饱和C13
4.45重量%的饱和C15
0.02重量%的单不饱和C15
0.20重量%的双不饱和C15
1.25重量%的饱和C17
19.10重量%的单不饱和C17
28.5重量%的双不饱和C17
0.60重量%的三不饱和C17
0.05重量%的饱和C19
1.25重量%的单不饱和C19
4.3重量%的其它
组分b:
25重量%的N-油酰基肌氨酸
组合物6:
组分a:
84重量%的1重量份的蒸馏的椰子脂肪酸和1重量份的妥尔油脂肪酸的混合物,其具有如下的烃链分布:
3.25重量%的饱和C7烃链
2.85重量%的饱和C9
25.65重量%的饱和C11
8.60重量%的饱和C13
4.45重量%的饱和C15
0.02重量%的单不饱和C15
0.20重量%的双不饱和C15
1.25重量%的饱和C17
19.10重量%的单不饱和C17
28.5重量%的双不饱和C17
0.60重量%的三不饱和C17
0.05重量%的饱和C19
1.25重量%的单不饱和C19
4.3重量%的其它
组分b:
16重量%的N-油酰基肌氨酸
3.对比捕集剂组合物
组合物7:
80重量%的妥尔油脂肪酸,其具有如下的烃链分布:
0重量%的饱和C7烃链
0重量%的饱和C9
0重量%的饱和C11
0重量%的饱和C13
0.30重量%的饱和C15
0.05重量%的单不饱和C15
0.40重量%的双不饱和C15
1.10重量%的饱和C17
30.30重量%的单不饱和C17
55.80重量%的双不饱和C17
1.20重量%的三不饱和C17
0重量%的饱和C19
2.50重量%的单不饱和C19
8.50重量%的其它
和
20重量%的N-油酰基肌氨酸
组合物8:
80重量%的蒸馏的椰子脂肪酸,其具有如下的烃链分布:
6.50重量%的饱和C7烃链
5.70重量%的饱和C9
51.30重量%的饱和C11
17.20重量%的饱和C13
8.60重量%的饱和C15
0重量%的单不饱和C15
0重量%的双不饱和C15
1.40重量%的饱和C17
7.90重量%的单不饱和C17
1.20重量%的双不饱和C17
0重量%的三不饱和C17
0.10重量%的饱和C19
0重量%的单不饱和C19
0.10重量%的其它
和
20重量%的N-油酰基肌氨酸
组合物9:
100重量%的妥尔油脂肪酸,其具有如下的烃链分布:
0重量%的饱和C7烃链
0重量%的饱和C9
0重量%的饱和C11
0重量%的饱和C13
0.30重量%的饱和C15
0.05重量%的单不饱和C15
0.40重量%的双不饱和C15
1.10重量%的饱和C17
30.30重量%的单不饱和C17
55.80重量%的双不饱和C17
1.20重量%的三不饱和C17
0重量%的饱和C19
2.50重量%的单不饱和C19
8.50重量%的其它
组合物10:
100重量%的1重量份的蒸馏的椰子脂肪酸和1重量份的妥尔油脂肪酸的混合物,具有如下的烃链分布:
3.25重量%的饱和C7烃链
2.85重量%的饱和C9
25.65重量%的饱和C11
8.60重量%的饱和C13
4.45重量%的饱和C15
0.02重量%的单不饱和C15
0.20重量%的双不饱和C15
1.25重量%的饱和C17
19.10重量%的单不饱和C17
28.5重量%的双不饱和C17
0.60重量%的三不饱和C17
0.05重量%的饱和C19
1.25重量%的单不饱和C19
4.3重量%的其它
4.浮选测试结果
实施例I:含有16.1%P2O5、47.9%SiO2、21.4%CaO和0.7%MgO的磷灰石矿石。
将390g份矿石样品在实验室不锈钢研磨机中以50rpm和66%固体研磨5分钟。这导致浮选进料的以下粒度分布:P50=17μm和P80=47μm。在研磨阶段完成后,将研磨的浆料转移到2.5L容量的浮选槽中,在其中通过添加适量的水将固体百分比调节至约15%。浮选装置是Denver D-12浮选机,叶轮速度设定为1100rpm。然后将浮选浆料按照指示的顺序分别用抑制剂硅酸钠(Na2SiO3,550g/t)和碳酸钠(Na2CO3,280g/t)调节4分钟和3分钟。接下来,在开始每次浮选测试之前,添加以1%溶液的形式新鲜制备的捕集剂混合物并且与浮选浆料调节3分钟。最后,将空气流速设定为2L/min,收集所得的泡沫12分钟。
浮选测试的结果表明,与参比组合物7和8相比,根据本发明的捕集剂组合物(1-3)显示出优异的浮选效率,特别是显著改进的矿物回收率。
用本发明组合物获得的P2O5品位略低于实验室实验中特别使用参比8所得到的那些。这种品位差异被认为是可忽略的,因为工业浮选设备典型地使较粗的精矿通过两个、三个或甚至四个清洁步骤。以这种方式,典型地提高最终精矿的品位。
实施例II:含有大约32%TiO2的钛铁矿矿石
从钛铁矿浮选设备的浮选进料流中收集大约1.2L样品。然后将1.2L样品(由大约1785g干矿石和750g水组成)转移到3.2L容量的浮选槽中。然后原样添加捕集剂并使用Denver D-12浮选设备调节10分钟,叶轮速度设定在1550rpm。然后通过加入1.0L工业用水,将浆料中的固体百分比从71%降至51%。此后,将空气流速设定为8.5L/min,并将所得的泡沫收集270秒。在所讨论的矿石的情况下,使用脂肪酸和石蜡作为捕集剂组合。结果如下所示。
浮选结果表明,脂肪酸捕集剂的1:1替代导致回收率增加5.1%与精矿品位轻微增加的组合。
实施例III:含有0.20%的WO3的白钨矿矿石
将研磨的矿石用抑制剂单宁(25g/t)、硅酸钠(350g/t)和碳酸钠(1000g/t)进行调节,然后通过添加所需量的NaOH溶液将浆料pH调节至pH 10。然后原样添加捕集剂并用浮选浆料调节2分钟,然后添加Clariant frother Flotanol 7026并调节另外的1分钟。此后,添加足够的水以将浮选槽中的固体百分比从调节步骤期间的60%降低至浮选步骤中的35%。空气流速现在设定为5L/min,并将所得的泡沫收集2分钟。
与对比产品(100%妥尔油脂肪酸捕集剂)相比,使用新的捕集剂混合物导致WO3品位的显著增加。此外,与对比妥尔油脂肪酸捕集剂的369g/t剂量相比,使用151g/t剂量的新捕集剂共混物获得了类似的WO3回收率值。
Claims (11)
1.用于非硫化物矿石的直接泡沫浮选的捕集剂组合物,其包含
a)50-99重量%的脂肪酸的混合物,和
b)1-50重量%的式(I)的肌氨酸的N-酰基衍生物
其中
R为具有7-21个碳原子的饱和或不饱和烃链,其中所述混合物包含10.0-35.0重量%的具有饱和C11烃基的脂肪酸、2.5-15.0重量%的具有饱和C13烃基的脂肪酸、10.0-25.0重量%的具有单不饱和C17烃基的脂肪酸和20.0-45.0重量%的具有双不饱和C17烃基的脂肪酸。
2.根据权利要求1所述的组合物,其中所述脂肪酸混合物包含具有以下的脂肪酸
1.0-6.5重量%的饱和C7烃基
1.0-4.0重量%的饱和C9
10.0-35.0重量%的饱和C11
2.5-15.0重量%的饱和C13
1.0-7.0重量%的饱和C15
0.0-1.0重量%的单不饱和C15
0.0-1.0重量%的双不饱和C15
0.5-2.0重量%的饱和C17
10.0-25.0重量%的单不饱和C17
20.0-45.0重量%的双不饱和C17
0.0-2.0重量%的三不饱和C17
0.0-1.0重量%的饱和C19
0.0-4.0重量%的单不饱和C19
0.0-7.0重量%的其它脂肪酸。
3.根据权利要求1和/或2所述的组合物,其中所述组分a)为0.3-1.7重量份的椰子油脂肪酸与1重量份的妥尔油脂肪酸的混合物。
4.根据权利要求1-3中任一项或多项所述的组合物,其中所述组分b)为N-油酰基肌氨酸。
5.根据权利要求1-4中任一项或多项所述的组合物,其中所述组分a)为80重量%的1重量份的椰子油脂肪酸和1重量份的妥尔油脂肪酸的混合物,和所述组分b)为20重量%的N-油酰基肌氨酸。
6.用于非硫化物矿物的直接泡沫浮选的方法,所述方法包括使根据权利要求1-5中任一项或多项所述的捕集剂组合物与非硫化物矿物的含水悬浮液接触并且使如此形成的矿浆起泡沫的步骤。
7.根据权利要求6所述的方法,其中所述非硫化物矿物为磷灰石。
8.根据权利要求6所述的方法,其中所述非硫化物矿物选自方解石、白钨矿、萤石、菱镁矿和重晶石。
9.根据权利要求6所述的方法,其中所述非硫化物矿物为钛铁矿。
10.根据权利要求6-9所述的直接泡沫浮选方法,其中添加的捕集剂组合物的量为每吨矿石介于100g和1000g之间的量。
11.根据权利要求1-5中任一项或多项所述的组合物的用途,作为捕集剂以每吨矿石介于100g和1000g之间的量用于非硫化物矿石的直接浮选。
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US20190194551A1 (en) | 2017-12-22 | 2019-06-27 | Clariant International, Ltd. | Synergized acetals composition and method for scavenging sulfides and mercaptans |
US11555140B2 (en) | 2017-12-22 | 2023-01-17 | Clariant International Ltd | Synergized hemiacetals composition and method for scavenging sulfides and mercaptans |
EP3956066A1 (en) | 2019-04-19 | 2022-02-23 | Nouryon Chemicals International B.V. | Collector compositions containing a n-acylated amino acid and process to treat non-sulfidic ores |
US20200391224A1 (en) * | 2019-06-17 | 2020-12-17 | Arr-Maz Products, L.P. | Reagent for sedimentary phosphate flotation |
RU2723787C9 (ru) * | 2019-11-29 | 2020-12-08 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Забойкальский государственный университет" (ФГБОУ ВО "ЗабГУ") | Способ переработки гипсосодержащих отходов производства борной кислоты |
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