Use of polyols for improving the reverse froth flotation process of iron ores
阅读说明：本技术 多元醇用于改进铁矿石的反向泡沫浮选工艺的用途 (Use of polyols for improving the reverse froth flotation process of iron ores ) 是由 M·克鲁尔 W·C·达西瓦 V·罗德斯 L·毕卡尔霍 于 2019-06-05 设计创作，主要内容包括：本发明涉及含两个或三个羟基的水可混容性多元醇用于改进包含至少一种式(I)的烷基醚胺和/或式(II)的烷基醚二胺的用于反向铁矿石浮选的捕集剂组合物的捕集剂性能的用途,R~1-(O-A)-NH_2(I)R~2-(O-A)-NH-R~3-NH_2(II)其中：R~1是含6-24个碳原子的烃基,R~2是含6-24个碳原子的烃基,R~3是含2-4个碳原子的脂族烃基A是含2-6个碳原子的亚烷基。(The invention relates to the use of water-miscible polyols containing two or three hydroxyl groups for improving the collector properties of collector compositions for reverse iron ore flotation comprising at least one alkyl ether amine of formula (I) and/or alkyl ether diamine of formula (II), R 1 ‑(O‑A)‑NH 2 (I)R 2 ‑(O‑A)‑NH‑R 3 ‑NH 2 (II) wherein: r 1 Is a hydrocarbon radical having 6 to 24 carbon atoms, R 2 Is a hydrocarbon radical having 6 to 24 carbon atoms, R 3 Is an aliphatic hydrocarbon radical A having 2 to 4 carbon atoms and is a radical having 2 to 6 carbon atomsAlkylene groups of carbon atoms.)
1. Use of a water-miscible polyol containing two or three hydroxyl groups (component B) for improving the collector performance of a collector composition (component a) for reverse iron ore flotation, said collector composition comprising at least one alkyl ether amine of formula (I) and/or an alkyl ether diamine of formula (II):
R1-(O-A)-NH2 (I)
R2-(O-A)-NH-R3-NH2 (II)
wherein:
R1is a hydrocarbon group having 6 to 24 carbon atoms,
R2is a hydrocarbon group having 6 to 24 carbon atoms,
R3is an aliphatic hydrocarbon group having 2 to 4 carbon atoms,
a is an alkylene group having 2 to 6 carbon atoms.
2. The use according to claim 1, wherein R1And R2Independently of one another, from 7 to 18 carbon atoms.
3. Use according to claim 1 and/or 2, wherein component a) is an alkyl ether amine of formula (I).
4. Use according to claim 1 and/or 2, wherein component a) is an alkyl ether diamine of formula (II).
5. Use according to claim 1 and/or 2, wherein component a) is a mixture of an alkyl ether amine of formula (I) and an alkyl ether diamine of formula (II).
6. Use according to one or more of claims 1 to 5, wherein R1And/or R2Independently of one another, is an aliphatic hydrocarbon residue.
7. Use according to one or more of claims 1 to 6, wherein R1And/or R2Is a linear or branched hydrocarbyl residue.
8. Use according to one or more of claims 1 to 7, wherein the alkyl ether amine (I) and/or alkyl ether diamine (II) is/are derived from a branched synthetic alcohol.
9. Use according to one or more of claims 1 to 8, wherein A is of formula-CH2-CH2Or formula-CH2-CH2-CH2-a group of (a).
10. Use according to one or more of claims 1 to 9, wherein R2Is of the formula-CH2-CH2Or formula-CH2-CH2-CH2-a group of (a).
11. Use according to one or more of claims 1 to 10, wherein the alkyl ether amine (I) and/or alkyl ether diamine has been partially neutralized.
12. Use according to claim 11, wherein the acid used for neutralizing the alkyl ether amine (I) and/or alkyl ether diamine (II) is a carboxylic acid containing 1-6 carbon atoms, preferably acetic acid.
13. Use according to one or more of claims 1 to 12, wherein R1And/or R2Is a branched alkyl residue.
14. Use according to claim 5, wherein the collector composition comprises the alkyl ether amine of formula (I) and the alkyl ether diamine of formula (II) in a weight ratio of 1:100 and 100: 1.
15. Use according to one or more of claims 1 to 14, wherein the water-miscible polyol contains 2 to 20 carbon atoms, more preferably 2 to 12 carbon atoms, most preferably 3 to 6 carbon atoms, and particularly preferably 3 to 5 carbon atoms.
16. Use according to one or more of claims 1-15, wherein the water-miscible polyol is selected from the group consisting of ethylene glycol, propylene glycol and glycerol.
17. The use of claim 16, wherein the water-miscible polyol is selected from the group consisting of ethylene glycol and glycerol.
18. Use according to one or more of claims 1-17, wherein the composition contains 50-99 wt% of the alkyl ether amine (I) and/or alkyl ether diamine (II), and 1-50 wt% of the water-miscible polyol (component B) is present.
19. The use according to one or more of claims 1 to 18, further comprising an inhibitor for iron ore.
20. Use according to one or more of claims 1-20, further comprising dispersants, chain extenders, foaming agents, defoamers, co-collectors and/or inhibitors.
21. Use according to one or more of claims 1-20, wherein the components a and B are added to the pulp in a total amount of 1-1,000g/to, relative to the amount of iron ore present.
22. Use according to one or more of claims 1-21, wherein the iron ore is selected from magnetite, hematite and goethite.
23. Use according to one or more of claims 1-22, wherein pH regulators, improvers, dispersants and/or inhibitors are present in the pulp.
24. Use according to one or more of claims 1 to 23, wherein the term "improving collector performance" means:
(i) the recovery of iron ore is increased when the alcohol is present, as compared to when no water-miscible polyol containing two or three hydroxyl groups is present;
(ii) a higher selectivity in removing silicates compared to when the water-miscible polyol is absent, meaning that the collector composition comprising the alcohol is capable of a higher proportion of iron retention and a higher proportion of silicates removal;
(iii) the amount of iron retained and the amount of silicate removed remain substantially unchanged when the temperature at which the use occurs is reduced to a temperature below 10 ℃, preferably as low as 5 ℃, or even below 5 ℃ in the presence of the alcohol, compared to the case where the amount of iron retained and silicate removed becomes worse in the absence of the water-miscible polyol;
(iv) the foam formed by the collector composition comprising the alcohol is lower in volume and collapses more quickly after separation from the flotation cell than when the water-miscible polyol is not present.
25. A method for improving the collector performance of a collector composition for enriching iron ore via reverse flotation of silicate-containing iron ore, the collector composition comprising at least one alkyl ether amine of formula (I) and/or alkyl ether diamine of formula (II):
R1-(O-A)-NH2 (I)
R2-(O-A)-NH-R3-NH2 (II)
wherein:
R1is a hydrocarbon group having 6 to 24 carbon atoms,
R2is a hydrocarbon group having 6 to 24 carbon atoms,
R3is an aliphatic hydrocarbon group having 2 to 4 carbon atoms,
a is an alkylene group having 2 to 6 carbon atoms,
the method comprises adding to the collector composition at least one water-miscible polyol containing two or three hydroxyl groups.
26. The process according to claim 25, wherein the component a and component B are added to the pulp in a total amount of 1-1,000g/to, relative to the amount of iron ore present.
27. The method of one or more of claims 25 and/or 26, wherein the iron ore is selected from the group consisting of magnetite, hematite, and goethite.
28. The method according to one or more of claims 25-27, wherein dispersants, chain extenders, foaming agents, defoamers, co-collectors and/or inhibitors are present in the pulp.
29. The method of one or more of claims 25-28, wherein the term "improving collector performance" refers to:
(i) the recovery of iron ore is increased when the alcohol is present, as compared to when no water-miscible polyol containing two or three hydroxyl groups is present;
(ii) a higher selectivity in removing silicates compared to when the water-miscible polyol is absent, meaning that the collector composition comprising the alcohol is capable of a higher proportion of iron retention and a higher proportion of silicates removal;
(iii) the amount of iron retained and the amount of silicate removed in the flotation process according to the second aspect when the temperature when performing the process is reduced to a temperature below 10 ℃, preferably as low as 5 ℃, or even below 5 ℃ in the presence of the alcohol remains substantially unchanged compared to the case where the amount of iron retained and silicate removed therein becomes worse in the absence of the water-miscible polyol;
(iv) the foam formed by the collector composition comprising the alcohol is lower in volume and collapses more quickly after separation from the flotation cell than when the water-miscible polyol is not present.
Examples
The percentages given refer to weight percentages unless otherwise indicated.
Materials used
The various collector compositions given in Table 1 were prepared from components A1-A5 and B1-B5 by mixing the components at 20 ℃ in the weight ratios given.
Table 1: composition and characterization of collector composition
Composition comprising a metal oxide and a metal oxide
A
B
CC1
80％A1
20％B3
CC2
70％A1
30％B3
CC3
90％A1
10％B3
CC4
95％A1
5％B3
CC5
80％A1
20％B1
CC6
80％A1
20％B2
CC7
80％A2
20％B3
CC8
80％A3
20％B3
CC9
80％A4
20％B3
CC10 (comparison)
80％A5
20％B3
CC11 (comparison)
100％A1
─
CC12 (comparison)
100％A2
─
CC13 (comparison)
100％A3
─
CC14 (comparison)
100％A4
─
CC15 (comparison)
100％A5
─
CC16 (comparison)
80％A1
20％B4
CC17 (comparison)
80％A1
20％B5
CC18 (comparison)
80％A1
20％B6
Comparative experiment, not according to the invention.
Collector compositions according to table 1 were tested in reverse iron ore flotation. Iron ore samples used in this study were characterized by chemical analysis and particle size analysis and the results are shown in table 2 (also referred to below as coarse iron ore).
Determination of SiO in ores by gravimetric method2And (4) content. The ore decomposes by acid attack (HCl), resulting in dissolution of metal oxides and metal hydroxides, and leaving behind insoluble SiO2As a residue.
The iron content in the ore was determined by titration, where the sample was decomposed by acid attack (HCl) by adding stannous chloride (SnC)l2) And mercuric chloride (HgCl) to reduce ferric iron to ferrous iron, and the iron content is determined by using potassium dichromate (K)2Cr2O7) And (4) carrying out titration measurement.
Particle size is determined by wet sieving according to ASTM E276-13, wherein sieves with different openings are used. The results of this analysis are given in table 2 below. P80 represents the diameter of the opening through which 80% of the particles pass; d50 represents the diameter of the particle below which 50 wt% of the sample mass is and above which 50 wt% of the sample mass is; the% 38 μm represents the percentage of particles smaller than 38 μm.
Table 2: characterization of crude iron ore for flotation experiments
Iron ore 1
Iron ore 2
Iron content
43.0％
41.2％
SiO2Content (wt.)
34.8％
41.0％
P80
97μm
137μm
D50
49μm
69μm
％-38μm
39.6％
22.0％
Flotation tests were carried out on a laboratory scale using a Denver Flotation Cell D12 apparatus at a temperature of about 25 ℃ according to the following procedure: a sample with 1.1 kg of the corresponding coarse iron ore was charged into a flotation cell of 1.5 liter volume and water was added to prepare a pulp with a solids content of 50 wt%. The agitator was set to a speed of 1100rpm and the slurry was homogenized for 1 minute. Then, inhibitor (NaOH alkalized corn starch in a starch to NaOH weight ratio of 5: 1) was added at a dosage rate of 600mg/kg relative to the dried ore. The pulp was conditioned for 5 minutes under stirring. The pH of the pulp is controlled and adjusted to 10.0 by further addition of NaOH, if necessary. The collector compositions according to Table 1 were added at a dose of 70mg/kg dry ore for crude iron ore 1 and 120mg/kg for crude iron ore 2. For ease of handling, the collector composition is applied as a1 wt% aqueous solution of the active ingredient. The collector was conditioned in the pulp for 1 minute. Then, the air flow was started and froth flotation was performed for 3 minutes. Floaters (tailings) and suppressants (enriched iron ore) were collected separately in separate bowls and dried in a laboratory oven. Then, the two samples (inhibited and floating) were analyzed for weight, SiO, according to the method described above2Content and iron content.
The results are given according to the following parameters:
yield (wt. -%): percentage of enriched ore (suppressor) relative to the total mass of the coarse iron ore
-SiO2Content (wt. -%): SiO present in enriched iron ores (suppressors)2The content of (a).
-fe.rec. (wt. -%): the weight ratio of the mass of iron recovered in the iron ore (suppressor) is enriched relative to the total mass of iron in the crude iron ore.
Table 3: results of flotation experiments with iron ore 1
Comparative experiment, not according to the invention.
Table 4: results of flotation experiments with iron ore 2
Comparative experiment, not according to the invention.
In the table, for example, comparative example 15 should be compared with example 11. It is apparent that in example 11, the yield is higher than in comparative example 15, SiO2Lower content and higher Fe recovery.
Evaluation of foaming behavior
The following procedure was used to evaluate the measurement of the foaming behaviour of the collector composition: a slurry consisting of 50g of coarse iron ore 1 and 50g of tap water was prepared in a graduated cylinder. A1 wt% active solution of a collector composition according to table 1 was added to the pulp at a dosage of 50mg/kg ore. The cylinder was tilted 15 times with an angle of 180 ° in 20 ± 2 seconds. The chronograph was started immediately after the last action. Foam height was measured immediately and after 30 seconds, 1 minute, 2 minutes, 3 minutes, 4 minutes, 5 minutes and 10 minutes. The results are given in table 6.
Table 6: collapse time of the obtained foam
The test results show that iron is enhanced by replacing a portion of the alkyl ether amine and/or alkyl ether diamine with a water-miscible polyolRecovery, i.e. a higher proportion of iron is retained. Simultaneously reducing SiO in concentrate2The content of (a). Together improving the selectivity of the process.
Although giving excellent iron recovery, the foams formed with the collector compositions according to the invention have a lower initial volume and subsequently collapse faster than foams formed by the use of alkyl ether amine (I) or alkyl ether diamine (II) in the absence of water-miscible polyols.
With the collector composition according to the invention, excellent performance is maintained in cold climates, whereas only the ether (di) amine loses its selectivity at low temperatures. This is particularly important in many large mining industries located in cold winter months, such as in the north states of the united states (e.g., michigan, minnesota) and in canada.
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