Title of Invention

"A NOVEL PROCESS FOR PREPARATION OF SELECTIVE AND POWERFUL MIXED FROTHER FOR COAL FLOATATION

Abstract

The present invention is provided with a process for preparation of a selective and powerful mixed frother for Coal flotation through blending mechanism of prime single frothing molecules comprising a two phase (air-water interface) floatation characterized parameter comprising a surface activity, a dynamic floatation index, a critical coalescence concentration and bubble size at ccc; a three phase (air-water solid interface) floatation characterized parameter comprising a selectivity, kinetics, size wise floatation performance; blending of pure single frothing molecules in the presence of a mixed chemical system of methyl isobutyl carbinol (MIBC) and polyglycol ether PPG-1000.

Full Text

FIELD OF APPLICATION The present invention relates to a process for preparation of a selective and powerful mixed frother for coal floatation. In particular, it relates to a process for screening frothing molecules for coal floatation under scientific guidelines, for coal benefication. BACKGROUND OF THE INVENTION The separation of fine particles of coal contained in coal slurry through the use of froth floatation processes is well known. Froth floatation processes involve introducing air into the coal slurry. The hydrophobic particles of coal are contacted with finely disseminated air bubbles such that the fine air bubbles become adhered to the hydrophobic coal particles. The particles carrying bubbles are then permitted to rise, forming froth on the surface of the slurry. The froth, containing the hydrophobic particles of coal, is skimmed from the surface of the coal slurry and collected, while rejecting any hydrophilic particles of impurities which do not adhere to the air bubbles and which remain suspended in the slurry. Floatation of coal fines has become Increasingly important as a separation and cleaning process where there is a lowering in both the particle size and grade of the coal being recovered from mining operations. The ability to remove the coal fines from coal washery or tailings is also advantageous in order to recover coal fines missed by other techniques of coal recovery. In order to improve the selectivity and recovery of the floatation process and enhance floating of the coal fines, various types of reagent have been developed for addition to the slurry. Frothers and collectors are two types of reagents which are commonly used in coal floatation. Floatation frothers are used to facilitate air dispersion into fine bubbles, and to stabilize the froth, According to Leja-Schulman's penetration theory frothers accumulate preferentially at the air-water interface and interact with collector molecules, adsorbed onto solid particles in the particle-to-bubble collision and attachment Effect of frothers on bubble size results from their ability to prevent bubble coalescence. The degree of bubble coalescence decreases with increasing frother concentration and at a particular concentration known as critical coalescence concentration (COC) for a frother, it reaches non coalescence environment Above the critical coalescence concentration there is very little effect on bubble size and to a large extent, the cell geometry affects the bubble size distribution. A successful frother must allow sufficient thinning of the liquid film between the colliding bubble and the particle so that attachment can take place in the time frame of the collision. Thinner liquid film enhances the bubble-particle attachment during collision process but it also increases the bubble-bubble coalescence. Thus a successful frother must achieve a delicate balance between these two competing processes and provide sufficient stability of the bubble/particles moiety and yet allow the weakly adhering or mechanically trapped particles of unwanted materials to escape with the draining liquid. Gravity is the main driving force for the drainage in froth phase. The surface gradient along the air-water interface creates the Gibbs-Marangoni effect that acts to retain the film thickness and prevent bubble coalescence. The froth stability also depends on, (a) particle size (finer particles stabilize froth), (b) wetting characteristics (particles having contact angle less than 90 degree stabilize froth and (c) shape of particles. Neutral frothers can be essentially divided into four groups. The first group consists of aromatic alcohols such as a-creasol and 2,3-xylenol. A second group is the alkoxy types such as triethoxy butane (TEB). The third group consists of aliphatic alcohols such as 2-ethyl hexanol, diacetone and methyl isobutyl carbinol (MIBC). In recent years, a fourth group of synthetic frothers consisting of polyethylene oxide (PEO), polypropylene oxide (PPO) and polybutylene oxide (PBO) types have been introduced into the market These chemicals may be presented by the general equation: It is generally known in industry that it is difficult to use a single pure frother that will effectively give good overall floatation performance for wide size distributed floatation feed (0.5 X 0.0 mm). It is due to some frothers are effective for coarse particles and others are good for floating ultra fine fractions. Attempts have been made to develop blended frothers for floating wide size distributed floatation feed. Examples of patents directed at improved frothers include U.S. Patent No. 4,582,596 issued April 15,1986, U.S. Patent No. 4,915, 825 issued April 10, 1990, U.S. Patent No. 4, 272, 364 issued June 09, 1981, U.S. Patent No. 4, 504, 385 issued March 12,1985, U.S. Patent No. 5, 304, 317 issued April 19,1994, U.S. Patent No. 3,710,939 issued January 16,1973, U.S. Patent No. 4, 606, 818 Issued August 19, 1986, U.S. Patent No. 4, 761, 223 issued August 02,1988, U.S. Patent No. 4,925,559 issued May 15,1990. In general practice, the frothers are screened under the general guidelines (price, availability, solubility in water, environment impact etc) and verification by laboratory and/or plant floatation data. It is generally accepted that adding a surface-active agent to water lowers the surface tension of the solution due to heteropolar nature of the reagent molecules. Thus, the surface tension of a solution is an Indication of the activity of a frother. Frothers that strongly tower the surface tension produce more stable froths. While the above conceptual picture is qualitatively correct, the use of surface tension measurements alone to screen frothers for application in floatation is limited. This is primarily due to the highly dynamic nature of the froth, especially in the presence of partides and turbulence. This situation Is not very different today and the terms "powerful" or "selective", which are used to characterize frothers, have intuitive rather than scientific meaning. There was therefore, a need for selection of selective and powerful mixed frother for coal floatation through blending mechanism of pure single frothing molecules. SUMMARY OF THE INVENTION The main object of the present invention is to provide a froth floatation process for beneficiating coat where coarse and ultrafine coal particles are selectively recovered in the presence of mixed chemicals system of methyl isobutyl carbinol (MIBC) and PPG-1000 (polygloycol ether). The process comprises characterizing of frothing molecules in two-phase (air- water interface) and three phase coal floatation. Scientific analysis provides linkage between two-phase frother classification Indices and coal floatation performance parameters. This novel process will facilitate in classification of frother and making suitable blended frother depending on the feed size distribution. The improvement in floatation process is governed by the novel approach for preparation of selective and powerful mixed frother for coal floatation through blending mechanism of pure single frothing molecules. This process contains characterization of frothing molecules in two-phase (air-water interface) and three phase coal floatation. Two phase frother characterization parameters are dynamic foamability index (OR), critical coalescene concentration (CCC), air bubble size distribution and surface activity and surfactants orientation at air- water interface. Selectivity, kinetics and size-wise floatation performance are three phase floatation characterization indices, Two phase fundamental frother characterization parameters are well correlated with floatation separation efficiency parameters. Surfactant molecules having loop and coil orientation at interface, high dynamic foamability index value, low critical coalescene concentration and high surface activeness are efficient for floating coarse particles. On the other hand molecules having vertical placement at air-water Interface, mono-fine bubble size, low dynamic foamability index and high critical coalescence concentration are selective for ultrafine coal particles. Mixed chemical systems of those frothing molecules are suitable coal floatation frother for broad size distributed floatation feed. Composition of methyl isobutyl carbinol (MIBC) and PPG-1000 in blended frotner depends on the ratio of ultrafine and coarse fraction in floatation feed. The methyl isobutyi carbinol can be present in an amount of 70 % and said PPG-1000 in an amount of 30 %. The blended frother of the present invention is used in a dosage ranging from between about 0.10 kg/t to about 0.20 kg/t of floatation feed coal. The blended frother (methyl isobutyi carbinol and PPG-1000) is capable in floating selectively of ultrafine and coarse coal particles. There is Improvement in 4 % clean coal yield and 1 % ash reduction with this blended frothing molecule. It also produces dry froth by means of reduction in froth moisture. The process for preparation of selective and powerful mixed frother for coal floatation through blending mechanism of pure single frothing molecules of the present invention helps in depth understanding of frother action in coal floatation process. This process comprises characterization of frothing molecules in two- phase (air-water interface) and three phase coal floatation. The floatation/surfactant molecules have loop and coil orientation at interface, high dynamic foamability index value, low critical coalescence concentration and high surface activeness are efficient for floating coarse particles. The molecules have vertical placement at air-water interface, mono-fine bubble size, low dynamic foamability index and high critical coalescence concentration are selective for ultrafine coal particles. The mixed chemical systems of the frothing molecules are suitable coal floatation frother for broad size distributed floatation feed. The blended frother of the present invention containing methyl isobutyl carblnol and PPG-1000 is showing improvement in 4 % dean coal yield and 1 % ash reduction. It also produces dry forth by means of reduction in froth moisture. Thus the present invention provides a process for preparation of a selective and powerful mixed frother coal floatation for coal benefication, comprising the steps of: characterizing frothing / surfactant molecules into two phase (air-water interface) flotation parameters and three phase flotation parameters; blending of pure single frothing / surfactant molecules In the presence of a mixed chemical system of methyl isobutyl carbinol (MIBC) and polyglycol ether PPG - 1000; and selectively recovering coarse and ultrafine coal particles from said mixed chemical system. BRIEF DESCRlPTION OF THE ACCOMPANYING DRAWINGS The invention can now be described in details with the help of the figures of the accompanying drawings in which: Rgure 1 shows schematic diagram of setup for testing frothability, foam stability and bubble size. Figure 2 shows the relationship between frother concentration and air bubble size. DETAILED DESCRIPTION The process of this invention for screening the frothing molecules and preparing blended chemicals results in an improved and efficient process for the recovery of coal values with enhanced recovery of coarse and ultrafine particles of the coal through addition of suitable frother in floatation. The invention of classification of frother is described here under sequential characterization techniques. The invention will become more readily apparent by explaining the process with example of PPG-1000 (Polygloycol ether family), methyl Isobutyl carbinol (Alcohol family) and Alpha-Terpinol (Alcohol family). Two-phases frother characterization Surface tension analysis Ring-Plate tensiometer is used to measure the surface tension of aqueous solutions at varying frother concentration at normal pH and room temperature. The surface tension decreases with Increasing frother concentration as molecutes adsorb at the liquid-air interface, Frother belonging to the polyglycol family decreases the surface tension more sharply compare to alcohol family frotners. It indicates that PPG-1000 is more surface active. Air-water interface affinity order of different frbthers at lower concentration is given below: PPG-1000>iAlpha-terplneol> MIBC For monodisperse nonionic surfactants, at constant pH, the adsorbed amount at air-water interface is given by the Gibbs adsorption isotherm where r is adsorption density, y is the static surface tension, T Is the absolute temperature, R is the ideal gas constant and C is the bulk frother concentration. The surface area occupied by a single molecule. Aexp, at the air-liquid interface is calculated as Where Av is the Avagdro number The equilibrium adsorption loading (I) and the adsorption area per molecule (AEXp) are presented in Table 1. As can be seen in Table 1, the adsorption loading of polyglycol ether (PPG-1000) is lower compared to alcohol family frothers. According to it, MIBC is required less area per molecule to adsorb at air/water interface compared to Alpha-Terpinol and PPG-1000. The molecular adsorption area of a methyl Isobutyl carbinol molecule and an Alpha-terpinol respectively are found to be 34 (A0)2 and 51 (A0)2. This alcohol family molecule ranges in chain length from approximately 6 A0 to 10 A0, with a diameter of approximately 2.0 A0. So these results are dose to the geometric dimensions of the hydrocarbon chain, indicating methyl isobutyl carbinol stands up at the air-water interface with -OH group oriented towards water phase and the hydrophobic chain towards air phase. From the equilibrium surface tension data, the molecular area of a PPG-1000 molecule is calculated 138 (A0)2. When ail the bond angles are taken into account, the length of the molecule is found to be 23 A0, while the diameter is 7.0 A0, giving a flat-lying molecular area of 162 (A0)2 whereas the vertical cross-sectional area is 39 (A0)2. The orientation of PPG-1000 at the air-water interface seems to be part way between completely lying down and completely standing up. It suggests the formation of loops and coiling up at the interface with PPG-1000 molecule. PPG-1000 has a much higher molecular weight (398) compared to methyl isobutyl carbinol (102) and this higher molecular weight may lead to a more viscous, and hence more stable, froth layer. There Is only one-OH group in methyl isobutyl carbinol and this group will interact with water molecules to form an oriented monolayer at the surface; but in PPG-1000, there are several oxygenated units in the molecular chain and each unit can interact with water molecules through hydrogen bonding, causing the molecules to tend to lie at the surface, possibly increasing viscosity of froth and hence foam stability. Foaming and stability A set-up is designed for the measurement of foamability and retention time as shown in Fig. 1. A graduated glass burette of 50 cm height and 2.5 cm diameter is fitted with a glass frit at the bottom and connected to a mercury manometer and air compressor. Experiments are carried out by talcing a known volume (15ml) of the reagent solution in the burrette and passing air to the solution at a fixed flow rate. Air is bubbled through a glass frit into the frother solution of known concentration to create foam. The steady state foam height (foamability) is measured as the distance between the liquid-foam interface and the top of the foam.After the newly formed foam has been stabilized and attained an equilibrium height (after approx 2-3 min), the steady state height is recorded. Since the cross sectional area of glass burette is same throughout Its length, the height is also measure of the volume of the foam generated by the air at a fixed air flow rate for a known frother concentration. The foam height increases with increasing air flow rate and frother concentration. PPG-1000 gives the highest froth volume and methyl isobutyl carblnol produces considerably lower foaming. For the testing of behavior of floatation frothers, the dynamic foamability index is measured. This measurement requires determination of the retention time (rt) from the slope of linear part of the dependence of the total gas volume (V) in solution and foam plotted versus gas flow rate (Q) for increasing frother concentration, which is accordance with Eq. (3). The retention time (rt) values are obtained then used to determine the dynamic foamability index (DFI), which is defined as the limiting slope of the retention time-concentration curve for C-> 0. Dynamic foamability index is defined as follows (Laskowski et at., 2003) Using the foamability data of methyl isobutyl carbinot concentration, PPG-1000 and Alpha-terpineol and Eq. (3), the foam retention time of the foamer at different concentration is calculated. Polyglycol ether frother (PPG-1000) has achieved maximum foaming performance at relatively low concentration. Methyl isobutyl carbinol is showing lower retention time, which results in poor frothing efficiency compare to other two frothers. The relative order of frother efficiency in terms of dynamic foamability index is given below: PPG-1000> Alpha--terpineol>MIBC Bubble size distribution The experimental set-up of foamability is used for imaging bubbles as shown in Figure 1. Bubble images in foam phase are captured using a CCD camera, which was connected to a personal computer where the visual information is stored and processed. The images captured during sampling are automatically processed using image analysis technique for measuring bubble size distribution. As can be seen from Figure 2, each curve is clearly divided into two concentration ranges, the low concentration range which can be approximated by a step linear fit and the flat horizontal portion at higher concentration. The intersection of the horizontal asymptote to the sauter bubble size-concentration curve with the step linear portion can easily be determined. This Is so called critical coalescence concentration (Cho and Laskowski, 2002; Grau et al. 2005). The general trend for all the investigated frothers are fairly similar, the bubble size decreases with increasing frother dosage, and at a particular concentration, the bubble size leveled off. Frother controls bubble size by reducing bubble coalescence in the cell and that coalescence is entirely prevented at concentration exceeding the critical coalescence concentration in a dynamic system. It is dear from Figure 2 that the critical coalescence concentration value is different for each type of frother and given in Table 2. At frother concentration exceeding the critical coalescence concentration value, the conditions In the cell can be defined as non-coalescing. PPG-1000 Is able to provide nonrcoalescing environment in floatation system at lowest concentration compared to other frothers belonging to alcohol family. Methyl isobutyl carbinol is the most effective frother in terms of bubble size reduction and the least effective one is PPG-1000, Frothers dont only hinder coalescence but also somehow affect bubble break-up under turbulent conditions. A representative minus 0.5 mm size semi bituminous floatation feed coal sample is taken in this investigation. Nature of coal sample is difficult to float Ash analysis is carried out according to ASTM D 3174-73 standard snowed that the sample contains 24.5 % ash. Size-wise weight and ash distribution analysis is conducted with a representative sample of the floatation feed. Floatation feed contains high percentage (20 %) of oversize fraction, namely -1+0.5 mm, having 23.5 % ash. Ultra size fraction (- 0.075 mm) is having maximum weight contribution in floatation feed content approx. 50 %. High-speed diesel oil is used as conventional collector. Three selected non-ionic surfactants are used as frother. Frother performance of these chemicals are characterized in term of selectivity, kinetics and size wise floatation performance as shown in Table 3. Methyl isobutyl carbinol is efficient selective frother compare to polyglycol frother PPG- 1000. Rate of recovery for polyglycol frother PPG-100G is faster compared to other alcohol frothers methyl isobutyl carbinol and Alpha-terpinonl. PPG-1000 is efficient in terms of recovery and grade for 0.5 X 0.075 mm fraction. But alcohol frother methyi isobutyl carbinol is very effective for ultrafine fraction (- 0.075 mm) In terms of reducing ash content and floating the coal particles. Smaller bubbles are obtained in the methyl isobutyl carbinol solution than in PPG-1000 solutions despite the same porous frit being used, as well as the PPG- 1000 solution having considerably lower surface tensions than the methyl isobutyl carbinol solutions at the similar concentrations. It follows that the adsorption for larger (and more surface active) molecules of PPG-1000 must be larger to prevent bubble from coalescence. Dynamic foamability index value indicates the dynamic stability of foam, In which bubbles do not easily coalesce. Critical coalescence concentration is a measure of minimum concentration of a given frother required to prevent coalescence. Table 2 shows that PPG-1000 is having high dynamic foamability index and low critical coalescence concentration and methyl isobutyl carbinol having low dynamic foamability index and high critical coalescence concentration value. From surface activity point, PPG-1000 is showing parallel (loop and coil) orientation at air-water interface. Methyl isobutyl carbinol is showing vertical configuration at interface. This information predicts that PPG-1000 is more efficient in preventing bubble coalescence and also producing more stable and viscous foam compare to frothers belonging to alcohol family. It reflects that higher water recovery from pulp phase to froth phase, more chance of floating coal and ash mineral particles and less drainage rate from froth phase of coal floatation with polyglycol frother (PPG-1000), PPG-1000 is showing faster kinetics and less selectivity due to entrainment through water compared to alcohol frothers. Methyl isobutyl carbinol is more efficient in bubble break-up process, means producing finer bubbles compared to polyglycol ether frother PPG-1000. From floatation practice, methyl isobutyl carbinol is very selective and appropriate for the floatation of ultrafine particles and PPG-1000 is better frother in terms of recovery and selectivity for coarse particles,. These two phase frother characterization indices and observations are well correlating with three phase floatation performance indexes for polyglycol ether and alcohol foaming molecules. The frother characterization indexes are summarized in Table 4. On the basis of observations obtained from frother classification process, PPG-1000 and methyl isobutyl carbinol are mixed in different composition. Floatation performance with mixed frother (PPG-1000 and methyl isobutyl carbinol) Is illustrated in Table 3. Blended frother is showing improvement in performance of recovery and grade of ultrafine and coarse coal fraction. So overall it is showing enhanced floatation efficiency. A good matching in critical coalescence concentration and dynamic foamability index values of PFG-1000 and methyl isobutyl cgrbinol is reported between this invention and work done since, despite the difference in experimental measuring systems. It also reflects that dynamic foamability index and critical coalescence coricentration can be material properties, for frothing molecules. The polyglycol ether and alcohol frothers are presenting good association between fundamental two phase frother characterization indices and coal floatation performance. REFERENCES CITED U.S. Patent No. 4, 582, 596 issued April 15,1986 U.S. Patent No. 4, 915, 825 issued April 10,1990 U.S. Patent No. 4, 272, 364 issued June 09,1981 U.S. Patent No. 4, 504, 385 issued March 12,1985 U.S. Patent No. 5,304, 317 issued April 19,1994 U.S. Patent No. 3,710,939 issued January 16,1973 U.S. Patent No. 4,606, 818 issued August 19,1986 U.S. Patent No. 4, 761, 223 issued August 02,1988 U.S. Patent No. 4, 925, 559 issued May 15,1990 Cho, Y.S., Laskowski, J.S., 2002. Bubble coalescence and Its effect on dynamic foamability. Can. X Chem. fcng. 80, 299-305. Grau, R.A., Laskowski, J.S., and Heiskanen, K., 2005. Effect of frothers on bubble size. Int J. Mineral Processing, 76(8), 225-233. Laskowski, J.S., Tlhone, T., Williams, P. and Ding, K., 2003. Fundamental properties of polyoxypropylene alkyl ether floatation frothers. Int. 3. Mineral Processing, 72, 289-299. WE CLAIM: 1. A process for preparation of a selective and powerful mixed frother for Coal flotation through blending mechanism of prime single frothing molecules comprising the step of: - a two phase (air-water interface) floatation characterized parameter comprising a surface activity, a dynamic floatation index, a critical coalescence concentration and bubble size at ccc; - a three phase (air-water solid interface) floatation characterized parameter comprising a selectivity, kinetics, size wise floatation performance; - blending of pure single frothing molecules in the presence of a mixed chemical system of methyl isobutyl carbinol (MIBC) and polyglycol ether PPG-1000; and characterized in that the two phase frother (air-water interface) having high DFI, low ccc and high surface activeness are efficient for floating coarse particles and a three phase frother (air-water solid interface) having parameter selectivity, kinetics, size-wise floatation performance, low DFI and high ccc are efficient for floating fine particles from the coal distribution. 2. The process as claimed in claim 1, wherein said two phase characterization parameters are dynamic foamability index (DFI), critical coalescence concentration (CCC), air-bubble size distribution and surface activity and surfactant orientation at air-water interface. 3. The process as claimed in claim 1, wherein said three phase characterization parameters are selectivity, kinetics and size-wise floatation performance. 4. The process as claimed in claim 2, wherein said flotation / surfactant molecules have a loop and coil orientation at the interface with high dynamic foamability index (DPI), low critical coalescence concentration values, and high surface, activeness for floating coarse particles. 5. The process as claimed in daim 2, wherein vertical placement at said air water interface, mono fine bubble size, low DFI and high CCC are selected for ultrafine coal partides. 6. The process as claimed in daim 1, wherein the composition of MIBC and PPG-1000 in the blended frother depends on ratio of ultrafine and coarse fractions in the flotation feed. 7. The process as claimed in daim 6, wherein said composition is 70 % MIBC and 30 % PPG -1000. 8. The process as claimed in preceding claims wherein said blended frother comprising MIBC and PPG - 1000 is capable of selectively floating ultrafine and coarse coal particles. 9. The process as claimed in preceding claims 6, wherein the dosage of said blended frother used is preferably between 0.10 kg/t to 0.20 kg/t of floatation feed coal. ABSTRACT A NOVEL PROCESS FOR PREPARATION OF A SELECTIVE AND POWERFUL MIXED FROTHER FOR COAL FLOATATION The present invention is provided with a process for preparation of a selective and powerful mixed frother for Coal flotation through blending mechanism of prime single frothing molecules comprising a two phase (air-water interface) floatation characterized parameter comprising a surface activity, a dynamic floatation index, a critical coalescence concentration and bubble size at ccc; a three phase (air-water solid interface) floatation characterized parameter comprising a selectivity, kinetics, size wise floatation performance; blending of pure single frothing molecules in the presence of a mixed chemical system of methyl isobutyl carbinol (MIBC) and polyglycol ether PPG-1000.

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