Abstract: A dispersed, emulsified and partially neutralized formulation of flotation collectors for separating alumina silicates or silicates from iron ore, said formulation comprises an amine component, selected from the group consisting of alkyl amines, alkyl diamines, and ether amines and mixtures thereof; at least one organic acid such as Acetic acid and/or mixtures thereof; emulsifying agent, selected from alkyl betaines or more preferably vicinyl betaines for having water solubility or alcohols and mixtures thereof; water.
FIELD OF THE INVENTION
00001. The present invention relates to a dispersed emulsified or partially neutralized or
formulation of flotation collectors having excellent selectivity separation of aluminasilicate or
silicate. The present invention also provides a process for using the formulation as cationic
aluminasilicate and silicate collectors in the reverse flotation of ores.
BACKGROUND OF THE INVENTION
2. While beneficiating the ore, processing plants generates huge quantities of ore
fines. These fines are being rejected at mines site due to their difficulty in processing and high
gangue content. These ore fines are detrimental to downstream processing due to their
compositions. Therefore, beneficiation of ore fines using froth flotation is required prior to the
downstream processing. Reverse flotation is a common process used for the beneficiation of these
ore fines. The presence of hydrated minerals along with aluminasilicate particularly kaolinites in
ore fines is difficult for flotation. Henceforth, the flotation collectors are to be more specific and
designed depending on mineralogical characteristics of ore body. The functional group of the
collector defines the selectivity for particular mineral depending on their binding mechanism and
the hydrophobic group of collector defines the floatability or collectability of particular mineral.
3. Alkyl amines, alkyl diamines, ether amines, ether diamines and polyamines have
been used as collectors for silica separation in a froth flotation process. Due to their poor solubility
in water, prior art disclosed various formulations of these compounds using solvent, dispersing or
emulsifying agent that make collector readily dispersible in water. US 2,816,870 disclose the use
of alkoxyalkanol and polyoxyethylene esters of mixed fatty acids and substituted oxazolines to
disperse the collector. US3034985, US3363758, US4168227, US4422928, US4319987,
US4732667 disclose the use of alkyl ether amines or diamines, primary amines and mixtures in
the form of acid salts. US3520820, CA1100239 discloses the emulsified form of ether amines and
diamines used in the froth flotation. US9403174B2, EP2017009A1 discloses the process of
formation of nanoemulsion collectors for reverse flotation of iron ore. US5540336, EP A0609257
discloses a process of flotation of silica from iron ore using collector comprises etheramines and
anionic or non-ionic surfactant. US8492572B2 describes the composition of fatty amine
carboxylate salt, water and carboxylic acid as collectors. WO 2016/065189 described the
composition of polyamidoamines and organic acid preferably acetic acid for froth flotation of
silicate minerals. In the above mentioned prior art, amines are selective particularly for the silica
and not for the aluminasilicates. These amines exhibit moderate selectivity and require in high
quantities for aluminasilicates particularly kaolinite separation. Alkyl guanidines described in
Patent Application No’s 816/KOL/2010, 1123/KOL/2015 by Tata Steel Ltd are difficult to
disperse due to their poor solubility (waxy solids) in water at room temperature. Due to its
solubility, large quantities of collector (1-1.5kg/ton) are used in the reverse flotation of iron ore.
In order to obtain maximum benefit of the collector, these collectors must be thoroughly dispersed
in aqueous phase of a flotation pulp. Therefore the more availability of collector for minerals such
as aluminasilicates or silicates will increase through surface adsorption and subsequently will
improve flotation performance. As only a mono-molecular layer of collector is required to render
the surface of mineral to hydrophobic, dispersion form of collector facilitates the monomolecular
adsorption and reduces the quantity of collector used in the flotation. Therefore, the present
invention of collector formulation can be used in a most efficacious manner and in small
quantities in a dispersed form than chemically identical non-dispersible collectors.
4. But the most of formulation used conventionally having difficulty to disperse due
to their poor solubility, as there are waxy solids in water at room temperature. Due to its solubility,
large quantities of collector (1-1.5kg/ton) are used in the reverse flotation of iron ore. In order to
obtain maximum benefit of the collector, these collectors must be thoroughly dispersed in aqueous
phase of a flotation pulp. Therefore the more availability of collector for minerals such as
aluminasilicates or silicates will increase through surface adsorption and subsequently will
improve flotation performance.
5. The present invention meets the long felt need by providing a monomolecular layer
of collector to render the surface of mineral to hydrophobic, dispersion form of collector facilitates
the monomolecular adsorption and reduces the quantity of collector used in the flotation.
6. The collector formulation as claimed hereinafter can be used in a most efficacious
manner and in small quantities in a dispersed form than chemically identical non-dispersible
collectors.
OBJECTS OF THE INVENTION
7. It is a general object of the present invention to provide a dispersed and partially
neutralized, dissolved formulation of flotation collectors to be used in reverse flotation of iron ore
fines.
8. Another object of the present invention is to provide a novel formulation, which
thoroughly disperses in aqueous phase of flotation pulp, thereby providing more availability of
collector through surface adsorption.
9. Yet another object of the present invention is to provide a novel formulation, which
render the surface of mineral to hydrophobic and thus reduces the quantity of the collector used in
the flotation.
10. Further object of the present invention is to provide a novel formulation, which act
as cationic collector for aluminasilicates and silicate mineral flotation.
11. Another object of the present invention is to provide a process of reverse flotation
of iron ore fines having high amount of goethite, aluminasilicate and silicate, when the formulation
is to be used to have excellent selectivity for aluminasilicates and silicate minerals.
12. Yet another object of the present invention is to provide a process of reverse
flotation of ore, where very small amount of the formulation such as 0.05 to 0.5 of non-dispersed
form of collector has used.
SUMMARY OF THE INVENTION
13. One or more drawbacks of conventional systems for a dispersed emulsified or
partially neutralized or formulation of flotation collectors having excellent selectivity separation
of aluminasilicate or silicate are overcome, and additional advantages are provided through the
method as claimed in the present disclosure. Additional features and advantages are realized
through the technicalities of the present disclosure. Other embodiments and aspects of the
disclosure are described in details herein and are considered to be part of the claimed disclosure.
14. The present invention relates to dispersed, dissolved, emulsified or partially
neutralized forms of flotation collectors and a method for making the same to use in reverse
flotation of iron ore fines. More particularly, this invention is applicable to the compositions
comprising a mixture of 1) an amine component, which is one or more compounds selected from
the group consisting of alkyl guanidine, alkyl biguandines, alkyl amines, alkyl diamines, alkyl
polyamines, ether amines and ether polyamines and mixtures thereof; 2) an organic acids or
mixtures thereof and/or 3) emulsifying agent, which is solvent or compounds selected from alkyl
betaines or alkoxy alkyl amines or alcohols and mixtures thereof. This invention also relates to a
process for using these formulations as cationic aluminasilicate and silica collectors in the reverse
flotation of ores, for example, as cationic aluminasilicate collectors in the reverse flotation of iron
ore. These formulations have excellent selectivity for the separation of aluminasilicate or silicate
minerals and require small quantities of collector than chemically identical non-dispersed
collectors used for the reverse flotation of aluminasilicates.
15. In accordance with a broad aspect of the invention, there is provided formulations
comprising amine compound consisting of alkyl guanidine and alkyl amines most preferably alkyl
monoamines or ether monoamines and mixtures thereof; an organic acid and emulsifying agent
such as protic solvent or alkyl betaines or alkoxy amines, alcohols and esters of fatty acids and
their mixtures; in the presence of water. This formulation consists of 1) one or more C6-C24,
preferably C7-C18, and most preferably C8-C12 alkyl guanidine and one or more C6-C24,
preferably C8-C12 alkyl amine or ether amine 2) an organic acid for partial neutralization of
amines to form salts to the extent of 30-70%, most preferably < 50% 3) an emulsifying agent,
preferably alcohols or alkyl betaines. The above said formulation contain up to 15% alkyl
guanidine, most preferably about 5% to 10%; alkyl monoamine or ether monoamine up to 10%,
most preferably about 0% to 5%; or their mixtures of salts, by weight and water is usually present
in an amount up to 98%, most preferably up to 95% by weight. A portion of the water is replaced
with a protic alcohol to form dissolved or dispersed stable formulation and present in an amount
up to 40%, by weight. The process of reverse flotation of ore to separate aluminasilicates using the
above mentioned formulation is developed. In the reverse flotation process, the formulation is
metered into the pulp at levels of from about 50 to about 1000 grams of alkyl guanidine per ton of
ore to be beneficiated, most preferably about 100 to about 500 grams.
16. Various objects, features, aspects, and advantages of the inventive subject matter
will become more apparent from the following detailed description of preferred embodiments.
17. It is to be understood that the aspects and embodiments of the disclosure described
above may be used in any combination with each other. Several of the aspects and embodiments
may be combined to form a further embodiment of the disclosure.
18. The foregoing summary is illustrative only and is not intended to be in any way
limiting. In addition to the illustrative aspects, embodiments, and features described above, further
aspects, embodiments, and features will become apparent by reference to the drawings and the
following detailed description.
BRIEF DESCRIPTION OF THE ACCOMPANYING DRAWINGS
19. The illustrated embodiments of the subject matter will be best understood by
reference to the drawings, wherein like parts are designated by like numerals throughout. The
following description is intended only by way of example, and simply illustrates certain selected
embodiments of devices, systems, and processes that are consistent with the subject matter herein,
wherein:
20. Fig. 1 illustrates the stable formulations of alkyl guanidine for (a) F2-F11 (b) F12
compositions.
21. Fig. 2 illustrates a reverse flotation process of iron ore to separate aluminasilicates
using collector formulations.
22. The figure depict embodiments of the disclosure for purposes of illustration only.
One skilled in the art will readily recognize from the following description that alternative
embodiments of the methods illustrated herein may be employed without departing from the
principles of the disclosure described herein.
DETAILED DESCRIPTION OF THE PRESENT INVENTION
000023. While the embodiments of the disclosure are subject to various modifications and
alternative forms, specific embodiment thereof have been shown by way the figures and will be
described below. It should be understood, however, that it is not intended to limit the disclosure
to the particular forms disclosed, but on the contrary, the disclosure is to cover all modifications,
equivalents and alternative falling within the scope of the disclosure.
24. It is to be noted that a person skilled in the art would be motivated from the present
disclosure to arrive at a dispersed and emulsified flotation collectors having excellent selectivity
for separation of aluminasilicate or silicate. Such formulation for evaluating the same may vary
based on combination of one or more ingredients. However, such modifications should be
construed within the scope of the disclosure. Accordingly, the drawings illustrate only those
specific details that are pertinent to understand the embodiments of the present disclosure, so as
not to obscure the disclosure with details that will be clear to those of ordinary skill in the art
having benefit of the description herein.
25. As used in the description herein and throughout the claims that follow, the
meaning of “a”, “an”, and “the” includes plural reference unless the context clearly dictates
otherwise. Also, as used in the description herein, the meaning of “in” includes “in” and “on”
unless the context clearly dictates otherwise.
26. The terms “comprises”, “comprising”, or any other variations thereof used in the
disclosure, are intended to cover a non-exclusive inclusion, such that a formulation that comprises
a list of components does not include only those components but may include other components
not expressly listed or inherent to such method, or assembly. In other words, one or more elements
in a system or device proceeded by “comprises…..a “does not, without more constraints, preclude
the existence of other elements or additional elements in the system, apparatus or device.
27. A description of an embodiment related to a dispersed, dissolved, emulsified or
partially neutralized formulation of flotation collectors. The present disclosure also provides a
method for using the formulation in reverse flotation of iron ore fines. The formulation is used as
cationic aluminasilicate and silica collectors in the reverse flotation of ores. These formulations
have excellent selectivity for the separation of aluminasilicate or silicate minerals and require small
quantities of collector than chemically identical non-dispersed collectors used for the reverse
flotation of aluminasilicates.
28. The formulation broadly comprises of:
1) an amine component, which is one or more compounds selected from the
group consisting of alkyl guanidine, alkyl biguandines, alkyl amines, alkyl diamines, alkyl
polyamines, ether amines and ether polyamines and mixtures thereof;
2) an organic acid such as acetic acid;
3) emulsifying agent, which is solvent or compounds selected from alkyl
betaines or alkoxy alkyl amines or alcohols and mixtures thereof in presence of water.
000029. The alkyl guanidine consists of C6-C24, preferably C7-C18 and most preferably
C8-C12 carbon atoms.
000030. The alkyl amine or ether amine consists of one or more C6-C24, preferably C8-C12
alkyl carbon atoms.
000031. The organic acid is used for partial neutralization of amines to form salts in quantity
of 30-70% or most preferably less than 50%.
000032. The emulsified formulation comprises alkyl betaines or vicinyl betaines with chain
length C2-C24, preferably C4-C18 and most preferably C4-C12. The above said emulsified
formulation contain up to 20% of vicinyl betaines, preferably about 5% to 15%; most preferably
about 2% to 10% by weight.
33. The compound selected from alkoxy form of alcohol or alkyl betaines esters of fatty
acid and mixtures are used as emulsifying agent or more particularly an emulsifier such as betaines,
preferably alkyl betaines or vicinyl betaines. Alkyl betaines or vicinyl betaines are zwitterionic
surfactants owing unique properties such as excellent water solubility used as emulsifier in
aqueous solutions.
34. These compounds rendered dispersible in flotation and can be used as collector in
reverse flotation.
35. The formulation of flotation collector comprises upto 15% or more particularly 5%
to 10%, alkyl guanidine. Upto 10% or more particularly 0% to 5%, alkyl monoamine or ether
monoamine or their mixtures of salts and 98% or most preferably 95% of water.
36. Further, the portion of the water is replaced with a protic alcohol to form dissolved
or dispersed stable formulation and present in an amount up to 40%, by weight.
37. The alkyl guanidine is described by general formula R1R2-NC(NH)NH2, alkyl
biguandines represented by general formula R1 & R2-NC(NH)-NH-C(NH)NH2 , alkyl amines,
alkyl diamines, alkyl polyamines, ether amines, ether diamines and ether polyamines and their
mixtures thereof. R1 can be from C8 to C12 and R2 can be any hydrocarbon chain or hydrogen.
000038. The amine compounds used for this process are given below:
40. In accordance, with an embodiment of the present invention, an experimental
procedure of synthesis of alkyl guanidine or more particularly octyl guanidine is provided.
41. The process of producing octyl guanidine comprises the steps of:
i) mixing of thiourea in demineralized water solution added to dimethyl sulphate
for a period of one hour to precipitate the solid at the temperature of 80°C, which maintained for
4 hour;
ii) addition of octyl amine to the white precipitate after cooling the same carefully
to avoid the excess foaming;
iii) heating of resultant mixture at a temperature of 60°C to 70°C for a period of 4
hour till the complete consumption;
iv) addition of water to precipitate the white solid, which is subjected to filtration,
washing and subsequent drying under vacuum for 1 hour to get the final product (octyl guanidine).
42. The white solid is subjected to characterization process by NMR spectroscopy.
43. The detailed experimental procedure is given below.
Experimental procedure: (telescopic reaction)
10g of Thiourea (0.131mol) in 75ml of demineralized water solution is added slowly to 6.2ml of
dimethyl sulphate (0.065mol) over a period of 1 hour during which small precipitation is observed
with addition. The temperature is raised to 80oC and maintained constant for 4h. A whiteprecipitate
formation is observed and the reaction mass is cooled to ambient temperature. Alkyl amine, for
example 26.6ml of octyl amine (0.144mol) is added very carefully to the obtained reaction mass
to avoid the excessive foaming during addition. The resultant mixture is heated at 60oC to 70oC
till the complete consumption of the substrate occurs (4h). After completion of the reaction, 60ml
water is added to precipitate white solid and then filtered, washed using pre-cooled water. The
resultant product is then dried under vacuum for 1h to achieve the desired compound of octyl
guanidine of 18.43g as a white solid with a yield of 80-90%.
Characterization by NMR
Similar to amines, alkyl guanidines and their derivatives have very low solubility in water; the
collector to be used successfully in flotation, it has to be formulated through partial neutralization
or emulsification to increase its solubility and dispersability in flotation. Partially neutralized
formulations of collector comprises alkyl guanidine and an organic acid or diacids in the form of
their salts along with water, most preferably alkyl guanidine, primary amines and mixtures in the
form of their salts in which acid is anionic radical and alkyl aminium ion is obviously the cationic
counterpart. These formulations improve the availability of collector to absorb on the mineral
surface by rendering in a dispersable form, so the resulting composition can be used in reverse
flotation of iron ore with low concentrations.
44. Alkyl vicinyl betaines is used as emulsifier in the flotation collectors.
45. This synthesis procedure of vicinyl betaines is given below:
Synthesis procedure:
Ethylene diamine is reacted with 4 equivalents of bromobutane in the presence of toluene solvent
at 0oC to ambient temperature. The reaction mixture is stirred for 2 hours at ambient temperature.
The obtained reaction mixture is neutralized with trimethylamine to form a trimethylamine salt.
The trimethylamine salt is dissolved by the addition of water and required compound is extracted
using the toluene solvent. Pure tetrabutylethane diamine compound is formed by evaporating the
toluene solvent. The obtained compound is treated with 2 equivalents of chloroacetic acid in
toluene at 90-100oC for 5 hours to obtain viscnyl betaine compound. Compound obtained as a pale
brown semi-solid with 80-90% yield.
000046. In accordance with another embodiment, a process for reverse flotation of iron ore
for separating aluminasilicates and silicates are also provided.
47. For lab-scale reverse flotation, standard OK flotation cell (Outokumpu) is used for
alumina and silica separation from iron ore. Initially, flotation cell is operated at maximum
impeller rotation to break the agglomerates and maintain dispersed state of iron ore slurry during
flotation. The air flow rate is measured using a rotameter set at 3 to 5 lpm for reverse flotation.
During conditioning of iron ore slurry, pH of slurry is adjusted and conditioned with reagents at
particular dosages to depress the iron minerals using starch and float aluminasilicates using above
mentioned formulation. Flotation parameters such as % solids, pH, and reagents dosage are
optimized for high selectivity and high collecting ability for alumina and silica (gangue). During
flotation, iron rich concentrate fraction is collected at the bottom of the cell and gangue rich reject
is collected in a froth launder. Both samples are analyzed for chemical analysis and the desired
concentrate is obtained at around 2-3% alumina with maximum yield.
48. Figure 2 illustrates the process of reverse flotation of iron ore in a pilot scale.
49. The iron ore slurry is conditioned in a mixing tank with the help of a pH modifier
to adjust the pH and a depressant such as causticized starch is added to the iron ore slurry and it is
pumped to the flotation circuit by gravity.
50. The collector formulation as claimed hereinafter is added to the iron ore slurry
before entering the flotation cell.
51. The number of points of collector addition in flotation cell is kept constant for all
the experiments. Froth from each flotation cell is collected in a common launder that treated as
reject and tailing from flotation circuit is collected in a tank that treated as concentrate. Both
samples are subjected to chemical analysis and the desired concentrate is obtained at around 2-3%
alumina with maximum yield. In lab and pilot scale flotation, the formulation is metered into the
pulp at levels of from about 50 to about 1000 grams of alkyl guanidine per ton of ore to be
beneficiated, most preferably about 100 to about 500 grams.
Examples 1
52. Different formulation of the formulation of flotation collector are provided in
Table 1 named as F1, F2, F3, F4, F5, F6, F7, F8, F9, F10, F11 and F12.
53. The composition of F1 to F12 is provided in Table 1.
000054. Table 1 shows examples of various stable formulations of alkyl guanidine.
Formulations from F2-F12 showed stable formulation of alkyl guanidine except F1 formulation
(acid salt without emulsifier). These alkyl guanidine formulations are being tested using different
organic acids at different concentrations. Different chain lengths of co-collectors such as alkyl
amines or ether amines are also tested. Besides, emulsified alkyl guanidine formulation with
synthesized alkyl betaines as emulsifier are also been tested. Figure 2 showed the stable
formulations of alkyl guanidine used for the reverse flotation of iron ore. It is been observed that
former formulations (F2-F11) of alkyl guanidine is in the dissolved state where as latter
formulation (F12) of alkyl guanidine is in the colloidal state. It is observed that non-stripped
alcohol alkyl guanidine exists in a stable formulation (F2-F11) than alcohol-stripped alkyl
guanidine (F1) and easy to formulate while synthesizing the compound without stripping or
isolation process. In these examples, monoamines are used due to their advantage for costing, easy
to formulate and high collecting ability for aluminasilicates than diamines. Compositions with
unsaturated mono amines or ether amines or poly amines are highly preferred than saturated
compositions to avoid the risk of precipitation. Compositions with branched alkyl chains of
monoamines are also preferred.
Examples 2
55. In lab scale, 0.5 to 1 kg of iron ore is treated with the formulation as mentioned. In
pilot scale flotation tests, 25 to 30 kg of iron ore is treated with alkyl guanidine formulations.
56. Table 2 provides the result of such flotation test and from this table, it can be
clearly seen that higher chain length alkyl amines alongwith formulation of alkyl guanidine
showed better separation of aluminasilicates from iron ore.
57. Hence, it can be concluded that in lab scale flotation tests, 0.5 – 1kg of iron ore is
treated with above mentioned formulations. Feed iron ore assay 3-4% alumina and 2-4% silica. In
pilot scale flotation tests, 25-30kg of iron ore is treated with alkyl guanidine formulations. From
the table 2, it is observed that higher chain length alkyl amines along with organic acid formulation
of alkyl guanidine showed better separation of aluminasilicates from iron ore. Most importantly,
the amount of collector used in the form of dispersed formulation is only about 0.05 to 0.5 times
of pure form of collector (1-1.5 kg/ton of ore) used for flotation. Consequently the guanidine
collector can be used in a most efficacious manner and in small quantities in a dispersed form than
chemically identical non-dispersable collectors.
58. Therefore, reverse flotation using these formulations provide higher selectivity to
achieve 61-63 Fe% concentrate with 70-80% yield at lower dosages of collector (0.05-0.5 kg/ton
of ore).
59. Each of the appended claims defines a separate invention, which for infringement
purposes is recognized as including equivalents to the various elements or limitations specified in
the claims. Depending on the context, all references below to the “invention” may in some cases
refer to certain specific embodiments only. In other cases, it will be recognized that references to
the “invention” will refer to subject matter recited in one or more, but not necessarily all, of the
claims.
60. Groupings of alternative elements or embodiments of the invention disclosed herein
are not to be construed as limitations. Each group member can be referred to and claimed
individually or in any combination with other members of the group or other elements found
herein. One or more members of a group can be included in, or deleted from, a group for reasons
of convenience and/or patentability. When any such inclusion or deletion occurs, the specification
is herein deemed to contain the group as modified thus fulfilling the written description of all
groups used in the appended claims.
Equivalents:
000061. With respect to the use of substantially any plural and/or singular terms herein,
those having skill in the art can translate from the plural to the singular and/or from the singular to
the plural as is appropriate to the context and/or application. The various singular/plural
permutations may be expressly set forth herein for sake of clarity.
62. It will be understood by those within the art that, in general, terms used herein, and
especially in the appended claims (e.g., bodies of the appended claims) are generally intended as
“open” terms (e.g., the term “including” should be interpreted as “including but not limited to”,
the term “having” should be interpreted as “having at least”, the term “includes” should be
interpreted as “includes but is not limited to”, etc.). It will be further understood by those within
the art that if a specific number of an introduced claim recitation is intended, such an intent will
be explicitly recited in the claim, and in the absence of such recitation no such intent is present.
For example, as an aid to understanding, the following appended claims may contain usage of the
introductory phrases “at least one” and “one or more” to introduce claim recitations. However, the
use of such phrases should not be construed to imply that the introduction of a claim recitation by
the indefinite articles “a” or “an” limits any particular claim containing such introduced claim
recitation to inventions containing only one such recitation, even when the same claim includes
the introductory phrases “one or more” or “at least one” and indefinite articles such as “a” or “an”
(e.g., “a” and/or “an” should typically be interpreted to mean “at least one” or “one or more”); the
same holds true for the use of definite articles used to introduce claim recitations. In addition, eve
it a specific number of an introduced claim recitation is explicitly recited, those skilled in the art
will recognize that such recitation should typically be interpreted to mean at least the recited
number (e.g., the bare recitation of “two recitations”, without other modifiers, typically means at
least two recitations, or two or more recitations).
63. The terminology used herein is for the purpose of describing particular
embodiments only and is not intended to be limiting of the present disclosure. It will be appreciated
that several of the above-disclosed and other features and functions, or alternatives thereof, may
be combined into other systems or applications. Various presently unforeseen or unanticipated
alternatives, modifications, variations, or improvements therein may subsequently be made by
those skilled in the art without departing from the scope of the present disclosure as encompassed
by the following claims.
64. While various aspects and embodiments have been disclosed herein, other aspects
and embodiments will be apparent to those skilled in the art. The various aspects and embodiments
disclosed herein are for purposes of illustration and are not intended to be limiting, with the true
scope and spirit being indicated by the following claims.
We claim:
1. A dispersed, emulsified and partially neutralized formulation of flotation collectors for
separating alumina silicates or silicates from iron ore, said formulation comprises:
i) an amine component, selected from the group consisting of alkyl amines, alkyl
diamines, and ether amines and mixtures thereof;
ii) at least one organic acid such as Acetic acid;
iii) emulsifying agent, selected from alkyl betaines or more preferably vicinyl betaines
for having water solubility or alcohols and mixtures thereof;
iv) water.
2. The formulation as claimed in claim 1, wherein said alkyl guanidine comprises one or
more C6-C24, preferably C7-C18 and most preferably C8-C12 carbon atoms.
3. The formulation as claimed in claim 1, wherein said alkyl amine or ether amine comprises
C6-C24, more preferably C8-C12 carbon atoms.
4. The formulation as claimed in claim 1, wherein said amine component comprises one or
more compounds selected from alkyl guanidine having a formula of R1R2-NC(NH)NH2, alkyl
biguandines having a formula of R1R2-NC(NH)-NH-C(NH)NH2 , alkyl amines, alkyl diamines,
alkyl polyamines, ether amines, ether diamines and ether polyamines and their mixtures thereof
R1 can be from C8 to C12 and R2 can be any hydrocarbon chain or Hydrogen.
6. The formulation as claimed in claim 1, wherein the quantity of all the ingredients are as
follows;
Alkyl Guanidine : Upto 15% or most preferably 5% to 10%
Primary Amine : Upto 10% or most preferably 2.5 to 6%
Water : 98% or more preferably 90-95%
Emulsifying Agent : Upto 20% or most preferably 5% to 15% or 2% to 10%
Organic Acid : Upto 5% most preferably 0.5% to 4%
7. A method for preparing alkyl guanidine comprises the steps of:
i) mixing of thiourea in demineralized water solution with dimethyl sulphate to
precipitate the solid at a suitable temperature;
ii) addition of alkyl amine (octyl amine) to the white precipitate to avoid the excess
foaming after cooling the same;
iii) heating of resultant mixture at a temperature of 60°C to 70°C for a period of 4 hour
till the complete consumption of all the ingredients;
iv) addition of water to precipitate the white solid, which is subjected to filtration,
washing and subsequent drying under vacuum for 1 hour to get the final product.
8. The process as claimed in claim 7, wherein thiourea solution is added to dimethyl sulphate
over a period of 1 hour at a temperature of 80°C, which kept constant for a duration of 4 hour.
9. The process as claimed in claim 7, wherein the mixture of white precipitate and alkyl
amine is heated at a temperature of 60°C to 70°C till the complete consumption of all the
ingredients takes place .
10. A method of reverse flotation of iron ore for separating aluminasilicate comprises the steps
of;
i) conditioning of iron ore slurry in a mixing tank by breaking the agglomerates with
adjustment of air flow rate and pH by using a pH modifier;
ii) pumping out of conditioned slurry to the flotation circuit, subjected to addition of
the collector formulation as claimed in claim 1;
iii) collection of froth in a common launder and tailing from flotation circuit, which is
collected in a tank as concentrate and subjected to different chemical analysis.
| Section | Controller | Decision Date |
|---|---|---|
| # | Name | Date |
|---|---|---|
| 1 | 202031006352-PROOF OF ALTERATION [04-08-2023(online)].pdf | 2023-08-04 |
| 1 | 202031006352-STATEMENT OF UNDERTAKING (FORM 3) [13-02-2020(online)].pdf | 2020-02-13 |
| 2 | 202031006352-IntimationOfGrant10-02-2023.pdf | 2023-02-10 |
| 2 | 202031006352-POWER OF AUTHORITY [13-02-2020(online)].pdf | 2020-02-13 |
| 3 | 202031006352-PatentCertificate10-02-2023.pdf | 2023-02-10 |
| 3 | 202031006352-FORM 1 [13-02-2020(online)].pdf | 2020-02-13 |
| 4 | 202031006352-Written submissions and relevant documents [01-12-2022(online)].pdf | 2022-12-01 |
| 4 | 202031006352-FIGURE OF ABSTRACT [13-02-2020(online)].pdf | 2020-02-13 |
| 5 | 202031006352-DRAWINGS [13-02-2020(online)].pdf | 2020-02-13 |
| 5 | 202031006352-Correspondence to notify the Controller [12-11-2022(online)].pdf | 2022-11-12 |
| 6 | 202031006352-FORM-26 [12-11-2022(online)].pdf | 2022-11-12 |
| 6 | 202031006352-DECLARATION OF INVENTORSHIP (FORM 5) [13-02-2020(online)].pdf | 2020-02-13 |
| 7 | 202031006352-US(14)-HearingNotice-(HearingDate-16-11-2022).pdf | 2022-10-06 |
| 7 | 202031006352-COMPLETE SPECIFICATION [13-02-2020(online)].pdf | 2020-02-13 |
| 8 | 202031006352-Proof of Right [09-07-2020(online)].pdf | 2020-07-09 |
| 8 | 202031006352-CLAIMS [04-03-2022(online)].pdf | 2022-03-04 |
| 9 | 202031006352-FER_SER_REPLY [04-03-2022(online)].pdf | 2022-03-04 |
| 9 | 202031006352-FORM 18 [11-07-2020(online)].pdf | 2020-07-11 |
| 10 | 202031006352-FER.pdf | 2021-10-18 |
| 11 | 202031006352-FER_SER_REPLY [04-03-2022(online)].pdf | 2022-03-04 |
| 11 | 202031006352-FORM 18 [11-07-2020(online)].pdf | 2020-07-11 |
| 12 | 202031006352-CLAIMS [04-03-2022(online)].pdf | 2022-03-04 |
| 12 | 202031006352-Proof of Right [09-07-2020(online)].pdf | 2020-07-09 |
| 13 | 202031006352-COMPLETE SPECIFICATION [13-02-2020(online)].pdf | 2020-02-13 |
| 13 | 202031006352-US(14)-HearingNotice-(HearingDate-16-11-2022).pdf | 2022-10-06 |
| 14 | 202031006352-DECLARATION OF INVENTORSHIP (FORM 5) [13-02-2020(online)].pdf | 2020-02-13 |
| 14 | 202031006352-FORM-26 [12-11-2022(online)].pdf | 2022-11-12 |
| 15 | 202031006352-Correspondence to notify the Controller [12-11-2022(online)].pdf | 2022-11-12 |
| 15 | 202031006352-DRAWINGS [13-02-2020(online)].pdf | 2020-02-13 |
| 16 | 202031006352-FIGURE OF ABSTRACT [13-02-2020(online)].pdf | 2020-02-13 |
| 16 | 202031006352-Written submissions and relevant documents [01-12-2022(online)].pdf | 2022-12-01 |
| 17 | 202031006352-FORM 1 [13-02-2020(online)].pdf | 2020-02-13 |
| 17 | 202031006352-PatentCertificate10-02-2023.pdf | 2023-02-10 |
| 18 | 202031006352-IntimationOfGrant10-02-2023.pdf | 2023-02-10 |
| 18 | 202031006352-POWER OF AUTHORITY [13-02-2020(online)].pdf | 2020-02-13 |
| 19 | 202031006352-STATEMENT OF UNDERTAKING (FORM 3) [13-02-2020(online)].pdf | 2020-02-13 |
| 19 | 202031006352-PROOF OF ALTERATION [04-08-2023(online)].pdf | 2023-08-04 |
| 1 | 202031006352searchE_31-08-2021.pdf |
| 1 | searchE_03-09-2021.pdf |
| 2 | 202031006352searchE_31-08-2021.pdf |
| 2 | searchE_03-09-2021.pdf |