EP0323323A1 - Andalusite beneficiation process - Google Patents
Andalusite beneficiation process Download PDFInfo
- Publication number
- EP0323323A1 EP0323323A1 EP88403286A EP88403286A EP0323323A1 EP 0323323 A1 EP0323323 A1 EP 0323323A1 EP 88403286 A EP88403286 A EP 88403286A EP 88403286 A EP88403286 A EP 88403286A EP 0323323 A1 EP0323323 A1 EP 0323323A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- andalusite
- flotation
- taken separately
- pulp
- carried out
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 229910052849 andalusite Inorganic materials 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000005188 flotation Methods 0.000 claims abstract description 81
- 239000007787 solid Substances 0.000 claims abstract description 36
- 239000012141 concentrate Substances 0.000 claims abstract description 27
- 150000001875 compounds Chemical class 0.000 claims abstract description 15
- 230000003750 conditioning effect Effects 0.000 claims abstract description 13
- 150000004760 silicates Chemical class 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 230000002045 lasting effect Effects 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 238000010790 dilution Methods 0.000 claims abstract description 4
- 239000012895 dilution Substances 0.000 claims abstract description 4
- 238000004537 pulping Methods 0.000 claims abstract description 4
- 239000008346 aqueous phase Substances 0.000 claims abstract description 3
- 230000005587 bubbling Effects 0.000 claims abstract description 3
- 150000008052 alkyl sulfonates Chemical class 0.000 claims description 11
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 9
- 239000011707 mineral Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 7
- 230000008030 elimination Effects 0.000 claims description 6
- 238000003379 elimination reaction Methods 0.000 claims description 6
- 239000004088 foaming agent Substances 0.000 claims description 6
- 150000003464 sulfur compounds Chemical class 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 239000011593 sulfur Substances 0.000 claims description 4
- 229910052717 sulfur Inorganic materials 0.000 claims description 4
- 150000002506 iron compounds Chemical class 0.000 claims description 3
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 claims 1
- 239000007864 aqueous solution Substances 0.000 claims 1
- 235000011007 phosphoric acid Nutrition 0.000 claims 1
- 150000003016 phosphoric acids Chemical class 0.000 claims 1
- 230000001105 regulatory effect Effects 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- -1 alkyl sulphonate Chemical compound 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 238000007792 addition Methods 0.000 description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 14
- 229910052593 corundum Inorganic materials 0.000 description 12
- 239000000047 product Substances 0.000 description 12
- 229910001845 yogo sapphire Inorganic materials 0.000 description 12
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 229910052742 iron Inorganic materials 0.000 description 9
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 5
- 238000004806 packaging method and process Methods 0.000 description 5
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- WVYWICLMDOOCFB-UHFFFAOYSA-N 4-methyl-2-pentanol Chemical compound CC(C)CC(C)O WVYWICLMDOOCFB-UHFFFAOYSA-N 0.000 description 4
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 4
- 229940045714 alkyl sulfonate alkylating agent Drugs 0.000 description 4
- INJRKJPEYSAMPD-UHFFFAOYSA-N aluminum;silicic acid;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O INJRKJPEYSAMPD-UHFFFAOYSA-N 0.000 description 4
- 235000013305 food Nutrition 0.000 description 4
- 239000010443 kyanite Substances 0.000 description 4
- 229910052850 kyanite Inorganic materials 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- 229920000151 polyglycol Polymers 0.000 description 3
- 239000010695 polyglycol Substances 0.000 description 3
- 229910052683 pyrite Inorganic materials 0.000 description 3
- 239000011028 pyrite Substances 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 150000004763 sulfides Chemical class 0.000 description 3
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 2
- 229910052626 biotite Inorganic materials 0.000 description 2
- 230000001143 conditioned effect Effects 0.000 description 2
- YGANSGVIUGARFR-UHFFFAOYSA-N dipotassium dioxosilane oxo(oxoalumanyloxy)alumane oxygen(2-) Chemical compound [O--].[K+].[K+].O=[Si]=O.O=[Al]O[Al]=O YGANSGVIUGARFR-UHFFFAOYSA-N 0.000 description 2
- 239000010423 industrial mineral Substances 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 229910052960 marcasite Inorganic materials 0.000 description 2
- 229910052627 muscovite Inorganic materials 0.000 description 2
- 229910052655 plagioclase feldspar Inorganic materials 0.000 description 2
- 229910052952 pyrrhotite Inorganic materials 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001447 alkali salts Chemical class 0.000 description 1
- 150000001412 amines Chemical group 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- JXLHNMVSKXFWAO-UHFFFAOYSA-N azane;7-fluoro-2,1,3-benzoxadiazole-4-sulfonic acid Chemical compound N.OS(=O)(=O)C1=CC=C(F)C2=NON=C12 JXLHNMVSKXFWAO-UHFFFAOYSA-N 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000011045 chalcedony Substances 0.000 description 1
- DVRDHUBQLOKMHZ-UHFFFAOYSA-N chalcopyrite Chemical compound [S-2].[S-2].[Fe+2].[Cu+2] DVRDHUBQLOKMHZ-UHFFFAOYSA-N 0.000 description 1
- 229910052951 chalcopyrite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 235000014571 nuts Nutrition 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000012264 purified product Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 230000033764 rhythmic process Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
- 239000012991 xanthate Substances 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/02—Froth-flotation processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/002—Inorganic compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/004—Organic compounds
- B03D1/012—Organic compounds containing sulfur
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/007—Modifying reagents for adjusting pH or conductivity
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2203/00—Specified materials treated by the flotation agents; Specified applications
- B03D2203/02—Ores
- B03D2203/04—Non-sulfide ores
Definitions
- the present invention which was carried out in the laboratories and mobile pilot installations of the company MINEMET RECHERCHE, relates to a process for the enrichment of an industrial mineral, andalusite, which is a particular form of aluminum silicate .
- This mineral is often associated with other silicates and sometimes even with some having the same formula.
- the flotation specialist already knows the reagents used to carry out a flotation of silicate compounds. These reagents are generally alkyl sulfonates, primary, secondary, tertiary amines or the salts of quaternary amines. It is also possible to use certain carboxylic acids, in particular those known under the name of fatty acids.
- one of the aims of the present invention is to provide a method for enriching andalusite by separation of the latter from its gangue and in particular from other natural silicates such as quartz, feldspar plagioclase, muscovite. , biotite.
- Another object of the present invention is to provide a process of the above type whose operating costs are as low as possible.
- Another object of the present invention is to provide a process which avoids having to work at a temperature above ambient and which therefore allows use of the process under variable climatic conditions and in particular that its economy is not affected by the summer-winter rhythm.
- step a) The two grinding and pulping operations of step a) can be carried out simultaneously in the case of wet grinding.
- step a) is carried out so that said compound has a d80 at most equal to 0.5 millimeter (rounded figure according to mathematical use).
- d x where x is between 1 and 100, is the smallest mesh allowing x% by weight of the product to pass.
- d80 is the smallest mesh allowing 80% of the product to pass through.
- said d80 be at most equal to 400 micrometers (a significant figure) and greater than the lower limit of flotation, which is of the order of 10 micrometers (a significant figure) .
- the pH plays a very important role; it is advantageously kept at a value less than 3 during step b) as well as in steps c), d) and e).
- the level of solid which, during steps b) and c), is preferably brought and maintained at a value at least equal to 50%.
- the first flotation carried out is insufficient to bring the content of andalusite to a value substantially greater than 90%.
- this content of 90% is a relatively low limit which is insufficient for certain commercial qualities and it is preferable that the content of andalusite is greater than 95%, even 98%.
- This can be remedied by performing following step e) the following step: f) rewashing the concentrate obtained in step e).
- This rewashing step is relatively classic per se in the enrichment process by flotation. In this specific case, it requires the addition of new quantities of flotation reagents, here the alkyl sulfonic acids and the alkali or ammonium salts.
- This rewashing of the concentrate can be carried out in several sub-steps and in several flotation cells arranged in cascade.
- a good guide for those skilled in the art to obtain good rewashability of the roughing concentrate is to stop this roughing flotation when only 80 to 95% of the andalusite is mounted in the form of scum.
- step c) The amounts of alkylsulfonate used in step c), and where appropriate in step f), are between 300 to 1,500 grams per tonne of ore processed.
- alkyl sulfonates used can be straight or branched chain and preferably have from 8 to 16 carbon atoms. They have at most two ramifications (three branches).
- BAYMIN CO 300 and CO 301 from BAYER
- SYNACTO 247 from PARAMINS
- Aero-Promoters of the 800 series from CYANAMID
- reagent 7723 from GERLAND
- R 231 from at FLOAT ORE Ltd.
- the pH of the pulp which may have changed during the addition of alkyl sulfonate, is brought to a value at most equal to 3 by addition of a strong mineral acid, in particular by means of an acid chosen from the group of strong hydrohalic acids (HCl), HBr, HI, sulfuric, nitric and phosphoric.
- a strong mineral acid in particular by means of an acid chosen from the group of strong hydrohalic acids (HCl), HBr, HI, sulfuric, nitric and phosphoric.
- the preferred temperature is therefore room temperature whatever the climatic conditions. It is perfectly possible to operate the process in the temperature range 10-30 ° C.
- step a) of grinding should be carried out so as to release at least 60% of the said ferric sulfur compounds, preferably 80 to 95%. A good compromise is often 90%.
- the duration of the proper flotation of said ferric sulfur compounds is equal to a value greater than the usual value of the sulfide flotation as skilled in the art can determine. As an indication, one chooses between 1.5 and 3 times said usual duration for this kind of compounds, all other things being equal.
- Deschamming is advantageously carried out by eliminating at least 75%, preferably at least 90%, of solid particles smaller than 50 micrometers, (a significant figure).
- the de-flaming be carried out as efficiently as possible, at the limit of the possibility of its means, which implies for these two techniques elimination of at least 95% of solid particles smaller than 50 micrometers.
- One of the surprising and advantageous aspects of the process according to the present invention is that it has been shown that the adsorption of the sulfonate on andalusite is reversible and that it is therefore possible to obtain andalusite without sulfonate by rinsing. in basic medium (greater than or equal to 9) of the flotation concentrate.
- the filtrate from step 2 can be recycled to step c) of the process, especially if the level of solid in operation 1 is greater than 1/2, preferably 3/4 (rounded figures).
- foaming agents for example those of the polyglycol type such as that sold under the trade name Aerofroth 65 of American Cyanamid (cf. example 5 ).
- Example 1 Description of the enrichment process at the pilot stage
- FIG. 1 constituting the rheogram of the process tested.
- a ball mill In a ball mill (A), the ore to be treated (1) and water (2) are introduced in an amount necessary to be at a mass concentration of solids of 30%.
- the ball load stepped from 10 to 40 millimeters, is calculated so as to deliver at the outlet of the mill a pulp (3) whose particle size is for 80% by weight less than 240 micrometers.
- the pulp (3) is then introduced into a double-blade reactor (B), brought to a solids concentration of 20 to 25% by the addition of water (4) and conditioned for 3 minutes in the presence of sulfuric acid in quantity sufficient to maintain a pH value of 5 and a dose of 100 grams per tonne of sulfide collector ore of the xanthat family.
- the pulp (5) is then conveyed to the flotation cells intended to collect the iron-bearing sulphides.
- This flotation step lasting 10 minutes, is carried out in several banks of MINEMET H 300 cells with 2 or 3 turbines (C) operating in series. Each turbine delivers 3.3 m3 / h of air.
- the number of turbines is advantageously brought to a value at least equal to 5.
- the introduction of 20 grams per tonne of surfactant (Methyl-isobutyl carbinol) at the start of the flotation makes it possible to recover in the form of foam the carrier sulfides iron and some ferric phyllitic minerals (6).
- the floated product represents 2 to 3% of the weight of the food.
- the rejection from this stage is pumped to a double-step screw classifier (or a cyclone) (D) in which the cut between the finest particles (less than 40 micrometers) which constitute the diluted rejection is effected by equivalence ( 8) and particles larger than 40 micrometers (9) which constitute the supply for the Andalusite flotation. This also thickens the pulp. (9) at a mass concentration value of solids of 70%.
- the pulp (9) which contains 91.5% of the weight of ore is then introduced into two double blade conditioners (E) operating in series.
- the second step is intended to condition for ten minutes the sulfonate introduced at the rate of 570 grams per tonne of general ore.
- the pulp (11) emerging from this second packaging is pumped to the flotation cells (F) which consist of a bank of two MINEMET cells of the H 450 type followed by two banks of three MINEMET cells of the H 300 type.
- Rejection rewash (16) also feeds the cells (F), which leads to a solids concentration close to 30%. This flotation lasts 9 minutes.
- the collected product (15) constitutes the final andalusite concentrate, while the solids which have not floated (16) return to the top of the draft flotation. ge (F).
- Al2O3 Fe2O3 Andal Al2O3 Fe2O3 Food 100 65.5 45.4 1.15 100 100 100 Pyrite flotation rejection 97.5 66.8 46.5 0.65 99.5 99.9 55.5 Schlamms 6.0 28.4 22.7 1.80 2.6 3.0 9.4 Andalusite flotation supply 91.5 69.4 48.1 0.58 96.9 96.9 46.1 Andalusite concentrate 65.0 89.2 59.2 0.59 88.5 84.8 33.3
- This example also illustrates the positive influence of de-flaming on the iron content of the product since this operation makes it possible to reduce the iron content of the product by 10%.
- steps A, B, C and D are identical to those described in Example 1.
- step E is identical to that of the previous example.
- step F water (12) is added so as to obtain a mass solids concentration of 25% in both cases.
- the progress of step F is modeled on that of Example 1.
- the floated product (13) is again collected during the rewashing step (G) after addition of water (15) making it possible to obtain a concentration close to 20%. Sulfuric acid is introduced during this step to maintain the pH at a value of 3.
- the flotation time and the material used are those of Example 1 for this same step.
- the rejection of this flotation (17) is not recycled while the concentrate (16) undergoes a second rewashing (H) after a new addition of water (18) to maintain a solids concentration of 20%.
- Sufficient sulfuric acid is also used to maintain the pH at 3 and 250 grams per tonne of sulfonate feed ore.
- the circuit is identical to that of the first rewash and allows the final Andalusite concentrate (19) to be collected and to eliminate a rejection from the second rewash (20).
- Tables 2.1 and 2.2 make it possible to compare the balances obtained for the two concentrations of the conditioning (the calculations are carried out with respect to the product (11). It can be seen that the mode of conditioning has little influence on the Andalusite roughing flotation. On the other hand, diluted packaging results in ineffective washes (little gain in content for a significant loss of Andalusite yield).
- FIG. 3 constituting the rheogram of the process tested.
- the pulp is conditioned in the presence of sulfuric acid in sufficient quantity to obtain a pH value of 5.
- 60 grams are also introduced per tonne of andalusite of sulfide collector (Amyl-xanthante of potassium: AXK).
- AXK Amyl-xanthante of potassium
- MIBC Metal-isobutyl carbinol
- 40 g / t of AXK and 15 g / t of MIBC are introduced in several doses.
- the concentrate obtained (7) consists of a pulp of sulphides.
- the rejection of this flotation (8) is again screened (D) at 63 micrometers in the presence of water (9).
- the sieving pass is a rejection (10).
- the rejection of sieving (11) is introduced into a flotation cell (E) previously described in (C) as well as water (12), which brings the concentration to 60% of solids.
- a 10-minute conditioning is then carried out in the presence of sufficient sulfuric acid to obtain a pH value of between 2 and 5 according to the tests and of an alkyl-sulfonate type collector at the rate of 350 grams per ton. Air is then introduced for 7 minutes so as to ensure the collection of andalusite and its overflow in the form of pulp (13).
- the pH is maintained at the desired value by a measurement / regulation system by servo pump.
- the characteristics of the andalusite concentrate, obtained after 7 minutes of flotation, are given in the following table for four different pH values.
- the weight yield is equal to the ratio of the weight of solid in the concentrate (3) to the weight of initial solid (1) expressed as a percentage.
- the Andalusite contents are those of the concentrate.
- Andalusite yields are the ratios of the Andalusite weight of the concentrate to that contained in the feed of the Andalusite flotation (11).
- step E of flotation for roughing Andalusite is also invariant.
- the only differences concerning roughing are the collector dose here equal to 1200 grams per tonne of ore in four additions, the flotation time (3.5 minutes for one test, 6 minutes for the other) and the dose d sulfuric acid introduced in sufficient quantity throughout the flotation to maintain a pH value of 3. It will also be noted that the ore (1) is different from that of Example 3.
- the concentrate (13) is introduced into a flotation cell (F) together with water (15), which brings the solid concentration to 30%.
- a conditioning is then carried out in the presence of sulfuric acid intended to maintain a pH value equal to 3.
- Air is then introduced for 5 minutes to collect the andalusite by overflow (16).
- this flotation are added, in two doses, 100 grams per tonne of ore coming from the collector of the alkyl sulfonate type as well as sulfuric acid in sufficient quantity to maintain the pH at the value of 3.
- the product which has not been collected is collected at the bottom of the cell (17).
- a polyglycol type foaming agent for example Aerofroth 65 from American Cyanamid
- Example 5 Comparison of the results of industrial roughing flotation with and without the addition of foaming agent.
- Example 2 The roughing flotation was carried out as in Example 1, with however a concentration of solid matter of approximately 20% and in cells of size clearly greater than that of the pilot since they had a capacity of approximately 4 m3 , each cell being equipped with four turbines.
- the first results showed a phenomenon of silting that it was possible to alleviate using systems known per se of automatic sand removal and somewhat complicated upstream recycling.
- This sanding phenomenon linked to a problem of change of scale, was resolved by adding a foaming agent of the polyglycol type (Aerofroth 65 from American Cyanamid).
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Paper (AREA)
- Catalysts (AREA)
- Saccharide Compounds (AREA)
- Treatment Of Water By Ion Exchange (AREA)
- Transition And Organic Metals Composition Catalysts For Addition Polymerization (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Manufacture And Refinement Of Metals (AREA)
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Abstract
Description
La présente invention, qui a été réalisée dans les làboratoires et les installations pilotes mobiles de la Société MINEMET RECHERCHE, a pour objet un procédé d'enrichissement d'un minéral industriel, l'andalousite, qui est une forme particulière de silicate d'aluminium.The present invention, which was carried out in the laboratories and mobile pilot installations of the company MINEMET RECHERCHE, relates to a process for the enrichment of an industrial mineral, andalusite, which is a particular form of aluminum silicate .
Ce minéral est souvent associé à d'autres silicates et parfois même à certains présentant la même formule.This mineral is often associated with other silicates and sometimes even with some having the same formula.
La séparation des silicates entre eux est une opération particulièrement délicate car elle mettrait souvent en jeu des mécanismes de flottation similaires. La flottation de tels minéraux nécessite souvent de longues études et un savoir-faire important car il est fréquent que des composés de même formule flottent très différemment. On peut citer comme exemples le quartz et la calcédoine. Cette difficulté se retrouve aussi pour d'autres minéraux non-silicatés : on peut citer la pyrite et la marcassite qui, bien qu'ayant une formule identique, en raison de leur réseau cristallin différent, voient, dans des conditions identiques, leur sélectivité vis-à-vis d'autres sulfures métalliques inversée lors des flottations.The separation of the silicates between them is a particularly delicate operation because it would often involve similar flotation mechanisms. The flotation of such minerals often requires long studies and significant know-how because it is common for compounds of the same formula to float very differently. Examples include quartz and chalcedony. This difficulty is also found for other non-silicate minerals: we can cite pyrite and marcasite which, although having an identical formula, because of their different crystal lattice, see, under identical conditions, their selectivity vis -to other metal sulfides reversed during flotation.
Le spécialiste en flottation connait d'ores et déjà les réactifs permettant de réaliser une flottation de composés silicatés. Ces réactifs sont en général les alcoylsulfonates, les amines primaires, secondaires, tertiaires ou les sels d'amines quaternaires. On peut également utiliser certains acides carboxyliques, notamment ceux connus sous le nom d'acides gras.The flotation specialist already knows the reagents used to carry out a flotation of silicate compounds. These reagents are generally alkyl sulfonates, primary, secondary, tertiary amines or the salts of quaternary amines. It is also possible to use certain carboxylic acids, in particular those known under the name of fatty acids.
Cependant, dans le cas de l'andalousite, compte tenu des marges peu élevées de ce minéral industriel, un grand nombre de techniques ne peuvent être appliquées en raison de leur coût. En outre, ce silicate d'aluminium est généralement extrêmement difficile à séparer de sa gangue elle-même silicatée. Parmi les minéraux constitutifs de cette gangue, on peut citer notamment le quartz, le feldspath plagioclase, la muscovite et la biotite. De plus, pour obtenir une qualité commerciale, il faut que la teneur en fer soit extrêmement faible.However, in the case of Andalusite, given the low margins of this industrial mineral, a large number of techniques cannot be applied in because of their cost. In addition, this aluminum silicate is generally extremely difficult to separate from its own silicate gangue. Among the minerals constituting this gangue, mention may in particular be made of quartz, plagioclase feldspar, muscovite and biotite. In addition, to obtain commercial quality, the iron content must be extremely low.
Un minéral voisin de l'andalousite, la kyanite (appelée parfois disthène), mais qui possède des propriétés distinctes de l'andalousite, a déjà fait l'objet d'études en vue d'un enrichissement par flottation. Toutefois, les auteurs de cette dernière étude sont parvenus à des conclusions différentes de celles de la recherche objet de la présente demande et d'autre part n'avaient conclu à la possibilité d'enrichissement que dans des conditions particulièrement onéreuses et peu sélectives vis-à-vis des silicates présents lorsqu'elles sont appliquées à la flottation de l'andalousite.A mineral close to andalusite, kyanite (sometimes called disthene), but which has properties distinct from andalusite, has already been studied for enrichment by flotation. However, the authors of this last study came to conclusions different from those of the research which is the subject of the present application and, on the other hand, only concluded that enrichment was possible under particularly expensive and not very selective conditions. vis-à-vis the silicates present when they are applied to the flotation of andalusite.
A titre de référence d'études sur les kyanites, on peut citer l'article de V.A. HAW "Kyanite in Canada" in The Canadian Mining and Metallurgical, Jan. 1954, pages 27-34, dans lequel l'auteur indique que les meilleurs résultats sont obtenus dans la zone de pH 4,0-4,5 à une température de 30°C. On retrouve des conditions pratiquement similaires dans l'article de J.S. BROWNING paru dans les Transactions of AIME en septembre 1969 (vol. 244, pages 283-287) sous le titre "Flotation of Southeastern Kyanite Ore" : pH de 3,7 à l'ébauchage et 3,9 au relavage et température de 27°C lors du conditionnement.As a reference for studies on kyanites, we can cite the article by V.A. HAW "Kyanite in Canada" in The Canadian Mining and Metallurgical, Jan. 1954, pages 27-34, in which the author indicates that the best results are obtained in the zone of pH 4.0-4.5 at a temperature of 30 ° C. Practically similar conditions are found in the article by JS BROWNING published in the Transactions of AIME in September 1969 (vol. 244, pages 283-287) under the title "Flotation of Southeastern Kyanite Ore": pH 3.7 to l roughing and 3.9 at rewashing and temperature of 27 ° C during packaging.
C'est pourquoi un des buts de la présente invention est de fournir un procédé d'enrichissement de l'andalousite par séparation de cette dernière d'avec sa gangue et notamment d'avec les autres silicates naturels tels que quartz, feldspath plagioclase, muscovite, biotite.This is why one of the aims of the present invention is to provide a method for enriching andalusite by separation of the latter from its gangue and in particular from other natural silicates such as quartz, feldspar plagioclase, muscovite. , biotite.
Un autre but de la présente invention est de fournir un procédé du type précédent dont les coûts opératoires soient aussi faibles que possible.Another object of the present invention is to provide a process of the above type whose operating costs are as low as possible.
Un autre but de la présente invention est de fournir un procédé qui évite d'avoir à travailler à une température supérieure à l'ambiante et qui donc permette une utilisation du procédé dans des conditions climatiques variables et notamment que son économie ne soit pas touchée par le rythme été-hiver.Another object of the present invention is to provide a process which avoids having to work at a temperature above ambient and which therefore allows use of the process under variable climatic conditions and in particular that its economy is not affected by the summer-winter rhythm.
Ces buts, ainsi que d'autres qui apparaîtront par la suite, sont atteints au moyen d'un procédé d'enrichissement de l'andalousite présente dans un composé en contenant, par séparation d'avec d'autres silicates par flottation pour obtenir un concentré dont la teneur en andalousite est supérieure à 90 %, caractérisé par le fait qu'il comporte au moins les étapes suivantes :
- a) broyage éventuel et mise en pulpe dudit composé contenant de l'andalousite
- b) pré-conditionnement dudit composé contenant de l'andalousite en maintenant le pH de la phase aqueuse de la pulpe à une valeur inférieure à 3,50, le taux de solide dans la pulpe étant supérieur à 30 % (un chiffre significatif) ;
- c) conditionnement pendant au moins dix minutes après addition d'un alcoyl sulfonate ;
- d) dilution éventuelle de ladite pulpe pour l'amener à un taux de solide compris entre 0,1 et 0,3 ;
- e) flottation par barbotage de bulles d'air calibrées de manière connue en soi, la flottation proprement dite durant au plus dix minutes.
- a) possible grinding and pulping of said compound containing andalusite
- b) preconditioning said compound containing andalusite while maintaining the pH of the aqueous phase of the pulp at a value less than 3.50, the level of solid in the pulp being greater than 30% (a significant figure);
- c) conditioning for at least ten minutes after addition of an alkyl sulfonate;
- d) optional dilution of said pulp to bring it to a solid content of between 0.1 and 0.3;
- e) flotation by bubbling air bubbles calibrated in a manner known per se, the flotation proper lasting at most ten minutes.
Lorsque, pour diverses raisons telles qu'une gangue basique ou addition de réactifs basiques, le pH s'élève au-dessus du maximum indiqué, il est préférable de réguler le pH dans les étapes c), d) et e) à une valeur inférieure à 4.When, for various reasons such as basic gangue or addition of basic reagents, the pH rises above the maximum indicated, it is preferable to regulate the pH in steps c), d) and e) to a value less than 4.
Les deux opérations de broyage et de mise en pulpe de l'étape a) peuvent être réalisées simultanément en cas de broyage humide.The two grinding and pulping operations of step a) can be carried out simultaneously in the case of wet grinding.
Il est préférable que le broyage de l'étape a) soit menée de manière que ledit composé présente un d₈₀ au plus égal 0,5 millimètre (chiffre arrondi selon l'usage mathématique).It is preferable that the grinding of step a) is carried out so that said compound has a d₈₀ at most equal to 0.5 millimeter (rounded figure according to mathematical use).
Rappelons que dx, où x est compris entre 1 et 100, est la plus petite maille laissant passer x % en poids du produit. Ainsi, le d₈₀ est la plus petite maille laissant passer 80 % du produit.Recall that d x , where x is between 1 and 100, is the smallest mesh allowing x% by weight of the product to pass. Thus, d₈₀ is the smallest mesh allowing 80% of the product to pass through.
Pour obtenir un bon rendement de la flottation, il est souhaitable ledit d₈₀ soit au plus égal à 400 micromètres (un chiffre significatif) et supérieur à la limite inférieure de la flottation, qui est de l'ordre de 10 micromètres (un chiffre significatif).To obtain a good flotation yield, it is desirable that said d₈₀ be at most equal to 400 micrometers (a significant figure) and greater than the lower limit of flotation, which is of the order of 10 micrometers (a significant figure) .
Pour obtenir une bonne sélectivité vis-à-vis des autres silicates et de la gangue en général, le pH joue un rôle très important ; il est avantageusement maintenu à une valeur inférieure à 3 pendant l'étape b) ainsi que dans les étapes c), d) et e).To obtain good selectivity vis-à-vis other silicates and gangue in general, the pH plays a very important role; it is advantageously kept at a value less than 3 during step b) as well as in steps c), d) and e).
Dans le domaine de la sélectivité, un autre paramètre joue un rôle non négligeable : le taux de solide, qui, lors des étapes b) et c), est de préférence porté et maintenue à une valeur au moins égale à 50 %.In the field of selectivity, another parameter plays a non-negligible role: the level of solid, which, during steps b) and c), is preferably brought and maintained at a value at least equal to 50%.
En général, la première flottation réalisée est insuffisante pour porter la teneur de l'andalousite à une valeur sensiblement supérieure à 90 %. En outre, cette teneur de 90 % est une limite relativement basse qui est insuffisante pour certaines qualités commerciales et il est préférable que la teneur en andalousite soit supérieure à 95 %, voire 98 %. Cela peut être pallié en réalisant à la suite de l'étape e) l'étape suivante :
f) relavage du concentré obtenu à l'étape e).In general, the first flotation carried out is insufficient to bring the content of andalusite to a value substantially greater than 90%. In addition, this content of 90% is a relatively low limit which is insufficient for certain commercial qualities and it is preferable that the content of andalusite is greater than 95%, even 98%. This can be remedied by performing following step e) the following step:
f) rewashing the concentrate obtained in step e).
Cette étape de relavage est "per se" relativement classique dans les processus d'enrichissement par flottation. Dans ce cas précis, elle nécessite l'addition de nouvelles quantités de réactifs de flottation, ici les acides alcoyl-sulfoniques et les sels alcalins ou d'ammonium. Ce relavage du concentré peut être réalisé en plusieurs sous-étapes et en plusieurs cellules de flottation disposées en cascade.This rewashing step is relatively classic per se in the enrichment process by flotation. In this specific case, it requires the addition of new quantities of flotation reagents, here the alkyl sulfonic acids and the alkali or ammonium salts. This rewashing of the concentrate can be carried out in several sub-steps and in several flotation cells arranged in cascade.
En outre, de manière extrêmement surprenante, il a été démontré, dans le cadre de la présente étude que le relavage n'était efficace que si l'étape de flottation proprement dite e), appelée par les hommes de métier "flottation d'ébauchage" était menée suffisamment rapidement, souvent au détriment du rendement poids.Furthermore, in an extremely surprising manner, it has been demonstrated, within the framework of the present study, that rewashing is only effective if the flotation step proper e), called by those skilled in the art "roughing flotation "was carried out quickly enough, often to the detriment of weight yield.
Un bon guide pour les hommes de métier pour obtenir une bonne relavabilité du concentré d'ébauchage est d'arrêter cette flottation d'ébauchage lorsque seulement 80 à 95 % de l'andalousite est montée sous forme d'écume.A good guide for those skilled in the art to obtain good rewashability of the roughing concentrate is to stop this roughing flotation when only 80 to 95% of the andalusite is mounted in the form of scum.
En général, une durée d'environ dix minutes (un chiffre significatif), comme indiqué précédemment, permet d'obtenir de bons résultats.In general, a duration of about ten minutes (a significant figure), as indicated above, allows good results to be obtained.
Les quantités d'alcoylsulfonate utilisées lors de l'étape c), et le cas échéant dans l'étape f), sont comprises entre 300 à 1 500 grammes par tonne de minerai traité.The amounts of alkylsulfonate used in step c), and where appropriate in step f), are between 300 to 1,500 grams per tonne of ore processed.
Les alcoylsulfonates utilisés peuvent être à chaîne linéaire ou ramifiée et ont de préférence de 8 à 16 atomes de carbone. Ils comportent au plus deux ramifications (soit trois branches). On peut utiliser notamment ceux vendus sous les noms commerciaux de BAYMIN CO 300 et CO 301 de chez BAYER, SYNACTO 247 de chez PARAMINS, les Aero-Promoters de la série 800 de chez CYANAMID, le réactif 7723 de chez GERLAND et le R 231 de chez FLOAT ORE Ltd.The alkyl sulfonates used can be straight or branched chain and preferably have from 8 to 16 carbon atoms. They have at most two ramifications (three branches). We can use in particular those sold under the trade names of BAYMIN CO 300 and CO 301 from BAYER, SYNACTO 247 from PARAMINS, the Aero-Promoters of the 800 series from CYANAMID, reagent 7723 from GERLAND and R 231 from at FLOAT ORE Ltd.
Avantageusement, le pH de la pulpe, qui peut avoir changé lors de l'addition d'alcoylsulfonate, est ramené à une valeur au plus égale à 3 par addition d'un acide minéral fort, notamment au moyen d'un acide choisi dans le groupe des acides halohydriques forts (HCl), HBr, HI, sulfurique, nitrique et phosphoriques.Advantageously, the pH of the pulp, which may have changed during the addition of alkyl sulfonate, is brought to a value at most equal to 3 by addition of a strong mineral acid, in particular by means of an acid chosen from the group of strong hydrohalic acids (HCl), HBr, HI, sulfuric, nitric and phosphoric.
Un des avantages de la présente invention est que, contrairement aux procédés connus pour des minéraux voisins, il n'est pas besoin de réguler la température. La température préférée est donc la température ambiante quelles que soient les conditions climatiques. Il est parfaitement possible de faire fonctionner le procédé dans l'intervalle de température 10-30°C.One of the advantages of the present invention is that, unlike the known methods for neighboring minerals, there is no need to regulate the temperature. The preferred temperature is therefore room temperature whatever the climatic conditions. It is perfectly possible to operate the process in the temperature range 10-30 ° C.
Une des contraintes importantes pour la commercialisation des andalousites est leur teneur en fer qui doit être aussi faible que possible et de préférence ne pas excéder 1,5 % exprimé en Fe₂O₃.One of the important constraints for the marketing of Andalusites is their iron content which must be as low as possible and preferably not exceed 1.5% expressed as Fe₂O₃.
Dans le cas où il y a du fer sous forme de composés sulfurés ferrifères, on réalise entre les étapes a) et b) une flottation, ou une éventuelle séparation magnétique dans le cas de la pyrrhotite, de ces derniers par des techniques connues en soi. Il est bien entendu que, pour que cette flottation soit efficace, il convient que l'étape a) de broyage est menée de manière à libérer au moins 60 % desdits composés sulfurés ferrifères, de préférence 80 à 95 %. Un bon compromis est souvent 90 %.In the case where there is iron in the form of iron-containing sulfur compounds, there is carried out between steps a) and b) a flotation, or a possible magnetic separation in the case of pyrrhotite, of the latter by techniques known per se. It is understood that, for this flotation to be effective, step a) of grinding should be carried out so as to release at least 60% of the said ferric sulfur compounds, preferably 80 to 95%. A good compromise is often 90%.
Au cours de l'étude qui a conduit à la présente invention, il a été montré de manière surprenante que pour réaliser une bonne élimination de composés sulfurés ferrifères, tels que la pyrite, la marcassite, la chalcopyrite, la pyrrhotine, il est préférable que la durée de la flottation proprement dite desdits composés sulfurés ferrifères soit égale à une valeur supérieure à la valeur usuelle de la flottation des sulfures telle que l'homme de métier peut la déterminer. A titre indicatif, on choisit entre 1,5 et 3 fois ladite durée usuelle pour ce genre de composés, toutes choses étant égales par ailleurs.During the study which led to the present invention, it was surprisingly shown that in order to achieve a good elimination of sulfur-containing iron compounds, such as pyrite, marcasite, chalcopyrite, pyrrhotite, it is preferable that the duration of the proper flotation of said ferric sulfur compounds is equal to a value greater than the usual value of the sulfide flotation as skilled in the art can determine. As an indication, one chooses between 1.5 and 3 times said usual duration for this kind of compounds, all other things being equal.
Il a été remarqué de manière surprenante qu'en agissant ainsi en utilisant les collecteurs classiques des sulfures, de préférence les xanthates, on flottait non seulement les composés sulfurés ferrifères mais aussi les composés phylliteux ferrifères.It has been surprisingly noticed that in doing so using the conventional sulfide collectors, preferably the xanthates, not only the sulfur-containing sulfur compounds are floated but also the phyllitous iron compounds.
Pour obtenir une bonne sélectivité, la présence de fines particules est gênante et ces dernières doivent être éliminées en réalisant un déschlammage avant l'étape b).To obtain good selectivity, the presence of fine particles is troublesome and these latter must be eliminated by carrying out a de-flaming before step b).
Le déschlammage est avantageusement réalisé par l'élimination d'au moins 75 %, de préférence d'au moins 90 %, des particules solides inférieures à 50 micromètres, (un chiffre significatif).Deschamming is advantageously carried out by eliminating at least 75%, preferably at least 90%, of solid particles smaller than 50 micrometers, (a significant figure).
Toutefois, suivant la technique de classification utilisée, de préférence une technique de classification par équivalence, il est préférable que le déschlammage soit mené de la manière la plus efficace possible, à la limite de la possibilité de ses moyens, ce qui implique pour ces deux techniques une élimination d'au moins 95 % des particules solides inférieures à 50 micromètres.However, depending on the classification technique used, preferably an equivalence classification technique, it is preferable that the de-flaming be carried out as efficiently as possible, at the limit of the possibility of its means, which implies for these two techniques elimination of at least 95% of solid particles smaller than 50 micrometers.
Un des aspects surprenants et avantageux du procédé selon la présente invention est qu'il a pu être montré que l'adsorbtion du sulfonate sur l'andalousite est réversible et qu'il est donc possible d'obenir de l'andalousite sans sulfonate par rinçage en milieu basique (supérieur ou égal à 9) du concentré de flottation.One of the surprising and advantageous aspects of the process according to the present invention is that it has been shown that the adsorption of the sulfonate on andalusite is reversible and that it is therefore possible to obtain andalusite without sulfonate by rinsing. in basic medium (greater than or equal to 9) of the flotation concentrate.
A titre indicatif, un tel rinçage peut être réalisé par la séquence d'opérations suivantes :
- 1. Conditionnement (repulpage) avec avec de la soude (NaOH) (1 kg/t de concentré)
pendant 5 mn (taux de solide supérieur à 10 %) ; - 2. Essorage sur tamis ;
- 3. Conditionnement (repulpage) à l'eau
pendant 5 mn ; - 4. Essorage sur tamis (les opérations 3
et 4 peuvent être renouvellées une ou plusieurs fois suivant le degré d'élimination du sulfonate désiré ;
- 1. Conditioning (repulping) with sodium hydroxide (NaOH) (1 kg / t of concentrate) for 5 min (solid content greater than 10%);
- 2. Spin on sieve;
- 3. Conditioning (plumping) with water for 5 min;
- 4. Spinning on a sieve (
3 and 4 can be repeated one or more times depending on the degree of elimination of the desired sulfonate;operations
Des essais de flottation standard sur le gateau repulpé à pH naturel (environ 9) et à 20 % de taux de pulpe environ n'entraîne pas d'andalousite dans la surverse démontrant ainsi l'absence d'adsorbtion résiduelle significative des alcoyl sulfonates sur l'andalousite. Il est à noter que cette technique de flottation permet d'abaisser la teneur de sulfonate dans les eaux mères et qu'une telle technique peut être utilisée pour éliminer une partie des alcoyl sulfonates.Standard flotation tests on the plump cake at natural pH (around 9) and at around 20% pulp rate do not cause andalusite in the overflow thus demonstrating the absence of significant residual adsorption of the alkyl sulfonates on the 'andalusite. It should be noted that this flotation technique makes it possible to lower the sulfonate content in the mother liquors and that such a technique can be used to remove part of the alkyl sulfonates.
On peut recycler le filtrat issu de l'étape 2 vers l'étape c) du procédé, surtout si le taux de solide dans l'opération 1 est supérieur à 1/2, de préférence à 3/4 (chiffres arrondis).The filtrate from
Par ailleurs, pour éviter les risques d'ensablement des installations industrielles de flottation, il est souhaitable d'ajouter des moussants, par exemple ceux du type polyglycol tels que celui vendu sous la marque commerciale Aerofroth 65 d'American Cyanamid (cf. exemple 5).Furthermore, to avoid the risk of siltation of industrial flotation installations, it is desirable to add foaming agents, for example those of the polyglycol type such as that sold under the trade name Aerofroth 65 of American Cyanamid (cf. example 5 ).
Les exemples non limitatifs suivants permettent à l'homme de métier de mieux appréhender les différents paramètres du procédé selon l'invention.The following nonlimiting examples allow those skilled in the art to better understand the different parameters of the process according to the invention.
On se reportera à la figure 1 constituant le rhéogramme du procédé testé.Reference will be made to FIG. 1 constituting the rheogram of the process tested.
Dans un broyeur à boulets (A), on introduit le minerai à traiter (1) et de l'eau (2) en quantité nécessaire pour être à une concentration massique en solides de 30 %. La charge de boulets, étagée de 10 à 40 millimètres, est calculée de façon à délivrer à la sortie du broyeur une pulpe (3) dont la granulométrie soit pour 80 % en poids inférieur à 240 micromètres. La pulpe (3) est alors introduite dans un réacteur à doubles pales (B), mise à une concentration en solides de 20 à 25 % par une addition d'eau (4) et conditionnée 3 minutes en présence d'acide sulfurique en quantité suffisante pour maintenir une valeur de pH de 5 et d'une dose de 100 grammes par tonne de minerai de collecteur de sulfures de la famille des xanthates. La pulpe (5) est ensuite acheminée vers les cellules de flottation destinées à collecter les sulfures porteurs de fer. Cette étape de flottation, d'une durée de 10 minutes, est réalisée dans plusieurs bancs de cellules MINEMET H 300 à 2 ou 3 turbines (C) fonctionnant en série. Chaque turbine délivre 3,3 m³/h d'air. Le nombre de turbines est avantageusement porté à une valeur au moins égale à 5. L'introduction de 20 grammes par tonne de tensio-actif (Méthyl-isobutyl carbinol) au début de la flottation permet de récupérer sous forme d'écumes les sulfures porteurs de fer ainsi que quelques minéraux phylliteux ferrifères (6). Dans cet exemple le produit flotté représente 2 à 3 % du poids de l'alimentation. Le rejet de cette étape est pompé vers un classificateur à vis à double pas (ou un cyclone) (D) dans lequel s'effectue par équivalence la coupure entre les particules les plus fines (inférieures à 40 micromètres) qui constituent le rejet dilué (8) et les particules de dimension supérieure à 40 micromètres (9) qui constituent l'alimentation de la flottation andalousite. Cette opération permet également l'épaississement de la pulpe (9) à une valeur de concentration massique en solides de 70 %.In a ball mill (A), the ore to be treated (1) and water (2) are introduced in an amount necessary to be at a mass concentration of solids of 30%. The ball load, stepped from 10 to 40 millimeters, is calculated so as to deliver at the outlet of the mill a pulp (3) whose particle size is for 80% by weight less than 240 micrometers. The pulp (3) is then introduced into a double-blade reactor (B), brought to a solids concentration of 20 to 25% by the addition of water (4) and conditioned for 3 minutes in the presence of sulfuric acid in quantity sufficient to maintain a pH value of 5 and a dose of 100 grams per tonne of sulfide collector ore of the xanthat family. The pulp (5) is then conveyed to the flotation cells intended to collect the iron-bearing sulphides. This flotation step, lasting 10 minutes, is carried out in several banks of MINEMET H 300 cells with 2 or 3 turbines (C) operating in series. Each turbine delivers 3.3 m³ / h of air. The number of turbines is advantageously brought to a value at least equal to 5. The introduction of 20 grams per tonne of surfactant (Methyl-isobutyl carbinol) at the start of the flotation makes it possible to recover in the form of foam the carrier sulfides iron and some ferric phyllitic minerals (6). In this example, the floated product represents 2 to 3% of the weight of the food. The rejection from this stage is pumped to a double-step screw classifier (or a cyclone) (D) in which the cut between the finest particles (less than 40 micrometers) which constitute the diluted rejection is effected by equivalence ( 8) and particles larger than 40 micrometers (9) which constitute the supply for the Andalusite flotation. This also thickens the pulp. (9) at a mass concentration value of solids of 70%.
La pulpe (9) qui contient 91,5 % du poids de minerai est alors introduite dans deux conditionneurs à doubles pales (E) fonctionnant en série.The pulp (9) which contains 91.5% of the weight of ore is then introduced into two double blade conditioners (E) operating in series.
Pendant le premier conditionnement, d'une durée de 6 minutes, on effectue un appoint d'eau (10) de façon à obtenir une concentration en solides de 50 % et une addition d'acide sulfurique en quantité suffisante pour maintenir une valeur de pH égale si possible à 2,8 et dans tous les cas inférieure à 3. La seconde étape est destinée à conditionner pendant une dizaine de minutes le sulfonate introduit à raison de 570 grammes par tonne de minerai tout-venant. La pulpe (11) sortant de ce second conditionnement est pompée vers les cellules de flottation (F) qui sont constituées d'un banc de deux cellules MINEMET du type H 450 suivi de deux bancs de trois cellules MINEMET du type H 300. Le rejet de relavage (16) alimente également les cellules (F), ce qui conduit à une concentration en solides voisine de 30 %. Cette flottation a une durée de 9 minutes. L'ensemble des turbines délivre 40 m³ d'air à l'heure. Au cours de la flottation d'ébauchage il est nécessaire de maintenir le pH à une valeur inférieure à 3 et d'introduire une dose de 570 grammes par tonne de sulfonate. Les produits non collectés (12), qui représentent 26,5 % du poids de départ, constituent le rejet de la flottation andalousite. L'andalousite est quant à elle collectée sous la forme d'une écume (13) qui alimente l'étage de relavage (G). Cette dernière étape, d'une durée de 9 minutes, est réalisée à une concentration massique de 20 %, ce qui implique une addition d'eau (14). Le pH est également maintenu à une valeur au plus égale à 3 par addition d'acide sulfurique et l'on ajoute 200 grammes par tonne de minerai tout-venant de sulfonate en tête des deux bancs de cellules MINEMET H 300 triples.During the first conditioning, lasting 6 minutes, water is added (10) so as to obtain a solids concentration of 50% and an addition of sulfuric acid in an amount sufficient to maintain a pH value. if possible equal to 2.8 and in all cases less than 3. The second step is intended to condition for ten minutes the sulfonate introduced at the rate of 570 grams per tonne of general ore. The pulp (11) emerging from this second packaging is pumped to the flotation cells (F) which consist of a bank of two MINEMET cells of the H 450 type followed by two banks of three MINEMET cells of the H 300 type. Rejection rewash (16) also feeds the cells (F), which leads to a solids concentration close to 30%. This flotation lasts 9 minutes. All of the turbines deliver 40 m³ of air per hour. During roughing flotation it is necessary to keep the pH below 3 and to introduce a dose of 570 grams per ton of sulfonate. Uncollected products (12), which represent 26.5% of the initial weight, constitute the rejection of Andalusite flotation. Andalusite is collected in the form of a scum (13) which feeds the rewashing stage (G). This last step, lasting 9 minutes, is carried out at a mass concentration of 20%, which involves the addition of water (14). The pH is also maintained at a value at most equal to 3 by the addition of sulfuric acid and 200 grams per tonne of general sulphonate ore are added to the top of the two banks of triple MINEMET H 300 cells.
Le produit collecté (15) constitue le concentré final d'andalousite, tandis que les solides qui n'ont pas flotté (16) retournent en tête de la flottation d'ébaucha ge (F).The collected product (15) constitutes the final andalusite concentrate, while the solids which have not floated (16) return to the top of the draft flotation. ge (F).
Dans ces conditions opératoires, et pour un minerai d'alimentation (1) titrant 45,4 % d'alumine et 1,15 % de fer exprimé en Fe₂O₃, on obtient un produit épuré qui titre 59,2 % d'alumine et moins de 0,6 % de Fe₂O₃ tout en récupérant plus de 88 % de l'andalousite contenue (voir tableau ci-dessous).
Cet exemple illustre également l'influence positive du déschlammage sur la teneur en fer du produit puisque cette opération permet de faire baisser de 10 % la teneur en fer du produit. Ceci résulte de l'utilisation du classificateur à vis (ou un cyclone) (D) qui permet l'élimination par élutriation de minéraux phylliteux ferrifères.This example also illustrates the positive influence of de-flaming on the iron content of the product since this operation makes it possible to reduce the iron content of the product by 10%. This results from the use of the screw classifier (or a cyclone) (D) which allows the elimination by elutriation of ferric phyllitous minerals.
L'influence de la concentration en solides de la pulpe lors du conditionnement qui précède la flottation andalousite sur le résultat de cette flottation est nettement mise en évidence par la comparaison de deux essais pilote effectués l'un avec un pourcentage massique de solides de 25 %, l'autre de 50 %.The influence of the pulp solids concentration during the conditioning which precedes the Andalusite flotation on the result of this flotation is clearly highlighted by the comparison of two pilot tests carried out, one with a mass percentage of solids of 25%. , the other 50%.
Le schéma de ces deux essais s'apparente d'assez près à celui de l'exemple précédant. On se réfèrera donc au rhéogramme de la figure 1 pour les étapes comprises entre A et E et au rhéogramme de la figure 2 pour les étapes suivantes (F, G et H).The scheme of these two tests is fairly similar close to that of the previous example. We will therefore refer to the rheogram of Figure 1 for the steps between A and E and to the rheogram of Figure 2 for the following steps (F, G and H).
Dans cet exemple, les étapes A, B, C et D sont identiques à celles décrites dans l'exemple 1. Par contre, il existe des différences dans les opérations suivantes. L'addition d'eau (10) est évidemment variable pour les deux essais décrits ici : les concentrations en solides de la pulpe lors du conditionnement sont de 25 % ou 50 %. Mis à part cette variation, l'étape E est identique à celle de l'exemple précédent. Avant l'étape de flottation d'ébauchage de l'andalousite (F), on ajoute de l'eau (12) de façon à obtenir une concentration en solides massique de 25 % dans les deux cas. Le déroulement de l'étape F est calqué sur celle de l'exemple 1. Le produit flotté (13) est à nouveau collecté au cours de l'étape de relavage (G) après addition d'eau (15) permettant d'obtenir une concentration voisine de 20 %. On introduit au cours de cette étape de l'acide sulfurique pour maintenir le pH à une valeur de 3. Le temps de flottation et le matériel utilisé sont ceux de l'exemple 1 pour cette même étape. Le rejet de cette flottation (17) n'est pas recyclé tandis que le concentré (16) subit un second relavage (H) après une nouvelle addition d'eau (18) pour maintenir une concentration en solides de 20 %. On utilise également de l'acide sulfurique en quantité suffisante pour maintenir le pH à 3 et 250 grammes par tonne de minerai d'alimentation de sulfonate. Le circuit est identique à celui du premier relavage et permet de collecter le concentré final d'andalousite (19) et d'éliminer un rejet du second relavage (20).In this example, steps A, B, C and D are identical to those described in Example 1. However, there are differences in the following operations. The addition of water (10) is obviously variable for the two tests described here: the solid concentrations of the pulp during conditioning are 25% or 50%. Aside from this variation, step E is identical to that of the previous example. Before the andalusite roughing flotation step (F), water (12) is added so as to obtain a mass solids concentration of 25% in both cases. The progress of step F is modeled on that of Example 1. The floated product (13) is again collected during the rewashing step (G) after addition of water (15) making it possible to obtain a concentration close to 20%. Sulfuric acid is introduced during this step to maintain the pH at a value of 3. The flotation time and the material used are those of Example 1 for this same step. The rejection of this flotation (17) is not recycled while the concentrate (16) undergoes a second rewashing (H) after a new addition of water (18) to maintain a solids concentration of 20%. Sufficient sulfuric acid is also used to maintain the pH at 3 and 250 grams per tonne of sulfonate feed ore. The circuit is identical to that of the first rewash and allows the final Andalusite concentrate (19) to be collected and to eliminate a rejection from the second rewash (20).
Les tableaux 2.1 et 2.2 permettent de comparer les bilans obtenus pour les deux concentrations du conditionnement (les calculs sont effectués par rapport au produit (11). On constate que le mode de conditionnement influe peu sur le flottation d'ébauchage andalousite. Par contre, le conditionnement dilué se traduit par une inefficacité des relavages (peu de gain de teneur pour une perte importante de rendement andalousite).
On se reportera à la figure 3 constituant le rhéogramme du procédé testé.Reference is made to FIG. 3 constituting the rheogram of the process tested.
Dans un broyeur à boulets de porcelaine A chargé de 50 boulets, on broie 1 kg de minerai (1) en présence d'eau (2) à 70 % poids de matières solides pendant 50 mi nutes. La pulpe obtenue (3) dont le d₈₀ est de 250 micromètres est tamisée en présence d'eau (4) sur un tamis (B) à maille 63 micromètres. Le refus de tamisage (5) est introduit dans une cellule de flottation (C) de marque MINEMET de 2,5 litres de capacité en présence d'eau (6), ce qui porte la concentration à 40 % poids de solides. Le passant de tamisage (6) est considéré comme rejet.In a porcelain ball mill A loaded with 50 balls, 1 kg of ore (1) is ground in the presence of water (2) at 70% by weight of solid matter for 50 minutes. nutes. The pulp obtained (3), the d₈₀ of which is 250 micrometers, is sieved in the presence of water (4) on a sieve (B) with a 63 micrometer mesh. The rejection of sieving (5) is introduced into a flotation cell (C) of the MINEMET brand with 2.5 liters capacity in the presence of water (6), which brings the concentration to 40% by weight of solids. The sieving pass (6) is considered as rejection.
Dans la cellule (C) on réalise un conditionnement de la pulpe en présence d'acide sulfurique en quantité suffisante pour obtenir une valeur de pH de 5. On introduit également 60 grammes par tonne d'andalousite de collecteur de sulfure (Amyl-xanthante de potassium : AXK). Après deux minutes, on introduit de l'air pour réaliser la flottation après avoir mis 8 grammes par tonne d'un tensio-actif (Méthyl-isobutyl carbinol : MIBC). Au cours de la flottation des sulfures, d'une durée de 10 minutes, on introduit en plusieurs doses 40 g/t d'AXK et 15 g/t de MIBC. Le concentré obtenu (7) est constitué d'une pulpe de sulfures.In cell (C), the pulp is conditioned in the presence of sulfuric acid in sufficient quantity to obtain a pH value of 5. 60 grams are also introduced per tonne of andalusite of sulfide collector (Amyl-xanthante of potassium: AXK). After two minutes, air is introduced to carry out the flotation after having put 8 grams per ton of a surfactant (Methyl-isobutyl carbinol: MIBC). During the 10-minute sulfide flotation, 40 g / t of AXK and 15 g / t of MIBC are introduced in several doses. The concentrate obtained (7) consists of a pulp of sulphides.
Le rejet de cette flottation (8) est de nouveau tamisé (D) à 63 micromètres en présence d'eau (9). Le passant de tamisage est un rejet (10). Le refus de tamisage (11) est introduit dans une cellule de flottation (E) précédemment décrite en (C) ainsi que de l'eau (12), ce qui porte la concentration à 60 % de solides. On réalise alors un conditionnement de 10 minutes en présence d'acide sulfurique en quantité suffisante pour obtenir une valeur de pH comprise entre 2 et 5 suivant les essais et d'un collecteur de type alkyl-sulfonate à raison de 350 grammes par tonne. On introduit ensuite de l'air pendant 7 minutes de façon à assurer la collection de l'andalousite et son débordement sous forme de pulpe (13). Au cours de la flottation le pH est maintenu à la valeur souhaitée par un système de mesure/régulation par pompe asservie.The rejection of this flotation (8) is again screened (D) at 63 micrometers in the presence of water (9). The sieving pass is a rejection (10). The rejection of sieving (11) is introduced into a flotation cell (E) previously described in (C) as well as water (12), which brings the concentration to 60% of solids. A 10-minute conditioning is then carried out in the presence of sufficient sulfuric acid to obtain a pH value of between 2 and 5 according to the tests and of an alkyl-sulfonate type collector at the rate of 350 grams per ton. Air is then introduced for 7 minutes so as to ensure the collection of andalusite and its overflow in the form of pulp (13). During flotation, the pH is maintained at the desired value by a measurement / regulation system by servo pump.
On introduit également deux autres doses égales de sulfonate représentant au total 700 grammes par tonne de minerai. Après la flottation, on vide la cellule du reste de la pulpe (14) contenant le produit n'ayant pas flotté.Two other equal doses of sulfonate are also introduced, representing a total of 700 grams per tonne of ore. After the flotation, the cell is emptied of the rest of the pulp (14) containing the product which has not fleet.
Les caractéristiques du concentré d'andalousite, obtenu après 7 minutes de flottation, sont données dans le tableau suivant pour quatre valeurs de pH différentes. Dans ce tableau le rendement poids est égal au rapport du poids de solide dans le concentré (3) sur le poids de solide initial (1) exprimé en pourcentage. Les teneurs andalousite sont celles du concentré. Les rendements andalousite sont les rapports du poids d'andalousite du concentré sur celui contenu dans l'alimentation de la flottation andalousite (11).
On constate la nette diminution de sélectivité lorsque l'on augmente le pH de la flottation andalousite. En particulier, pour la valeur de pH couramment utilisée pour la kyanite, la sélectivité est insuffisante.There is a marked decrease in selectivity when the pH of the Andalusite flotation is increased. In particular, for the pH value commonly used for kyanite, the selectivity is insufficient.
Le rhéogramme du procédé est identique à celui de l'exemple 3 pour ce qui concerne les opérations A, B, C et D. Le principe de l'étape E de flottation d'ébauchage de l'andalousite est également invariant. Les seules différences concernant l'ébauchage sont la dose de collecteur égale ici à 1 200 grammes par tonne de minerai en quatre additions, le temps de flottation (3,5 minutes pour un essai, 6 minutes pour l'autre) et la dose d'acide sulfurique introduite en quantité suffisante pendant toute la flottation pour maintenir une valeur de pH de 3. On notera également que le minerai (1) est différent de celui de l'exemple 3.The rheogram of the process is identical to that of Example 3 with regard to operations A, B, C and D. The principle of step E of flotation for roughing Andalusite is also invariant. The only differences concerning roughing are the collector dose here equal to 1200 grams per tonne of ore in four additions, the flotation time (3.5 minutes for one test, 6 minutes for the other) and the dose d sulfuric acid introduced in sufficient quantity throughout the flotation to maintain a pH value of 3. It will also be noted that the ore (1) is different from that of Example 3.
A la suite de cette flottation, le concentré (13) est introduit dans une cellule de flottation (F) ainsi que de l'eau (15), ce qui porte la concentration en solides à 30 %. On réalise alors un conditionnement en présence d'acide sulfurique destiné à maintenir une valeur de pH égale à 3. On introduit alors de l'air pendant 5 minutes pour collecter l'andalousite par débordement (16). Au cours de cette flottation sont ajoutés, en deux doses, 100 grammes par tonne de minerai tout-venant du collecteur du type alkyl sulfonate ainsi que de l'acide sulfurique en quantité suffisante pour maintenir le pH à la valeur de 3. A la fin de cette opération, on recueille dans le fond de la cellule le produit n'ayant pas été collecté (17).Following this flotation, the concentrate (13) is introduced into a flotation cell (F) together with water (15), which brings the solid concentration to 30%. A conditioning is then carried out in the presence of sulfuric acid intended to maintain a pH value equal to 3. Air is then introduced for 5 minutes to collect the andalusite by overflow (16). During this flotation are added, in two doses, 100 grams per tonne of ore coming from the collector of the alkyl sulfonate type as well as sulfuric acid in sufficient quantity to maintain the pH at the value of 3. At the end of this operation, the product which has not been collected is collected at the bottom of the cell (17).
Les résultats des deux essais portant sur l'influence du temps de flottation d'ébauchage sur l'efficacité du relavage sont donnés dans le tableau suivant.
On constate qu'avec un ébauchage court le relavage permet un gain de teneur sans perte de rendement. A l'inverse, lorsque l'ébauchage dure 6 minutes, le relavage ne permet quasiment pas de gain de teneur malgré une perte importante de rendement.It can be seen that with short roughing, rewashing allows a gain in content without loss of yield. Conversely, when roughing lasts 6 minutes, rewashing hardly allows any gain in content despite a significant loss of yield.
Exemple montrant qu'au cours de la flottation industrielle, on a tout intérêt à ajouter au début de la flottation d'ébauchage de l'andalousite 1/20 à 1/10 kg/t (chiffres arrondis) d'un moussant de type polyglycol (par exemple Aerofroth 65 d'American Cyanamid) pour éviter les phénomènes d'ensablement.Example showing that during industrial flotation, it is best to add at the start of the roughing flotation of
De même la flottation d'ébauchage pour des concentrations en solide de la pulpe inférieures à 25 voire à 20 % joue également un rôle dans la lutte contre les phénomènes d'ensablement.Similarly, roughing flotation for pulp solid concentrations of less than 25 or even 20% also plays a role in the fight against the phenomena of silting up.
La flottation d'ébauchage a été réalisée comme dans l'exemple 1, avec toutefois une concentration en matière solide d'environ 20 % et dans des cellules de taille nettement supérieure à celle du pilote puisqu'elles avaient une capacité d'environ 4 m³, chaque cellule étant équipée de quatre turbines.The roughing flotation was carried out as in Example 1, with however a concentration of solid matter of approximately 20% and in cells of size clearly greater than that of the pilot since they had a capacity of approximately 4 m³ , each cell being equipped with four turbines.
Les premiers résultats ont montré un phénomène d'ensablement qu'il était possible de pallier à l'aide de systèmes connus en soi de désensablage automatique et d'un recyclage en amont quelque peu compliqué. Ce phénomène d'ensablement, lié à un problème de changement d'échelle, a été résolu en ajoutant un agent moussant du type polyglycol (Aerofroth 65 d'American Cyanamid).The first results showed a phenomenon of silting that it was possible to alleviate using systems known per se of automatic sand removal and somewhat complicated upstream recycling. This sanding phenomenon, linked to a problem of change of scale, was resolved by adding a foaming agent of the polyglycol type (Aerofroth 65 from American Cyanamid).
Les résultats sont résumés dans le tableau ci-après :
Claims (18)
f) relavage du concentré obtenu à l'étape e).6. Method according to claims 1 to 5, taken separately, characterized in that it comprises, after step e) the following step:
f) rewashing the concentrate obtained in step e).
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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AT88403286T ATE85537T1 (en) | 1987-12-24 | 1988-12-22 | ANDALUSITE PROCESSING PROCESSES. |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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FR8718135 | 1987-12-24 | ||
FR8718135A FR2625115B1 (en) | 1987-12-24 | 1987-12-24 | METHOD FOR ENRICHING ANDALUSITY |
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EP0323323A1 true EP0323323A1 (en) | 1989-07-05 |
EP0323323B1 EP0323323B1 (en) | 1993-02-10 |
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EP88403286A Expired - Lifetime EP0323323B1 (en) | 1987-12-24 | 1988-12-22 | Andalusite beneficiation process |
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US (1) | US4900431A (en) |
EP (1) | EP0323323B1 (en) |
AT (1) | ATE85537T1 (en) |
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CA (1) | CA1311864C (en) |
DE (1) | DE3878440T2 (en) |
FR (1) | FR2625115B1 (en) |
ZA (1) | ZA889630B (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103111364A (en) * | 2013-03-06 | 2013-05-22 | 合肥万泉非金属矿科技有限公司 | Technology of extracting quartz and feldspar from gangue |
Families Citing this family (10)
Publication number | Priority date | Publication date | Assignee | Title |
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FR2661845B1 (en) * | 1990-05-09 | 1992-09-04 | Damrec Snc | PROCESS FOR ENRICHING ANDALOUSITY BY FLOTATION. |
US5338338A (en) * | 1992-09-22 | 1994-08-16 | Geobiotics, Inc. | Method for recovering gold and other precious metals from carbonaceous ores |
US5364453A (en) * | 1992-09-22 | 1994-11-15 | Geobiotics, Inc. | Method for recovering gold and other precious metals from carbonaceous ores |
DE102006010939A1 (en) * | 2006-03-09 | 2007-09-13 | Clariant International Limited | Flotation reagent for silicates |
DE102006019561A1 (en) * | 2006-04-27 | 2007-10-31 | Clariant International Limited | Use of an amine compound as collectors in silicate flotations, for the reverse flotation of silicate containing minerals from e.g. iron ore, for the cleaning of silicate sand and in the flotation of quartz, glimmer, feldspar and muscovite |
CN102029225A (en) * | 2010-09-25 | 2011-04-27 | 徐霖 | Method for separating feldspar and quartz by two stages of mixing and flotation |
CN102476076A (en) * | 2010-11-25 | 2012-05-30 | 何建庭 | New purpose of primary and secondary alkyl sodium sulfonate |
CN108927291B (en) * | 2017-05-24 | 2022-10-25 | 中蓝连海设计研究院有限公司 | Combined collector for andalusite ore separation and preparation method and application thereof |
CN112007763B (en) * | 2019-12-16 | 2022-03-22 | 中蓝连海设计研究院有限公司 | Combined collecting agent for andalusite ore separation and preparation method and application thereof |
CN112058500B (en) * | 2020-07-29 | 2022-03-11 | 中钢集团马鞍山矿山研究总院股份有限公司 | Beneficiation method for comprehensively utilizing magnetite concentrate flotation desulfurization foam products |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3117924A (en) * | 1960-12-16 | 1964-01-14 | Armour & Co | Flotation process to produce separate aluminum silicates and zircon concentrates from a heavy mineral beach sand concentrate |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2238439A (en) * | 1939-07-25 | 1941-04-15 | Hercules Powder Co Ltd | Froth flotation process |
US2305502A (en) * | 1941-04-09 | 1942-12-15 | Phosphate Recovery Corp | Concentration of kyanite |
US2289741A (en) * | 1941-04-09 | 1942-07-14 | Phosphate Recovery Corp | Concentration of kyanite |
US2326807A (en) * | 1942-02-06 | 1943-08-17 | Minerals Separation North Us | Concentration of kyanite |
US3214018A (en) * | 1962-10-08 | 1965-10-26 | Feldspar Corp | Froth flotation of micaceous minerals |
US4213851A (en) * | 1978-08-11 | 1980-07-22 | Occidental Petroleum Corporation | Flotation separation of glass from a mixture of comminuted inorganic materials using hydrocarbon sulfonates |
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1987
- 1987-12-24 FR FR8718135A patent/FR2625115B1/en not_active Expired - Lifetime
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1988
- 1988-12-21 AU AU27424/88A patent/AU609362B2/en not_active Expired
- 1988-12-21 CA CA000586584A patent/CA1311864C/en not_active Expired - Lifetime
- 1988-12-21 US US07/287,164 patent/US4900431A/en not_active Expired - Lifetime
- 1988-12-22 DE DE8888403286T patent/DE3878440T2/en not_active Expired - Fee Related
- 1988-12-22 AT AT88403286T patent/ATE85537T1/en not_active IP Right Cessation
- 1988-12-22 EP EP88403286A patent/EP0323323B1/en not_active Expired - Lifetime
- 1988-12-27 ZA ZA889630A patent/ZA889630B/en unknown
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3117924A (en) * | 1960-12-16 | 1964-01-14 | Armour & Co | Flotation process to produce separate aluminum silicates and zircon concentrates from a heavy mineral beach sand concentrate |
Non-Patent Citations (3)
Title |
---|
CHEMICAL ABSTRACTS, vol. 66, no. 5, 30 janvier 1967, page 1990, résumé no. 20617x, Columbus, Ohio, US; A.S. JOY et al.: "Flotation of silicates. I. Proposals for classification according to their flotation response", & INST. MINING MET., TRANS. SECT. C75(712), C75-C80(1966) * |
THE CANADIAN MINING AND METALLURGICAL BULLETIN, vol. XLVII, nos 501-512, 1954, pages 27-35, The Canadian Institute of Mining and Metallurgy, Montreal, Quebec, CA; V.A. HAW: "Kyanite in Canada" * |
TRANSACTIONS OF MINING ENGINEERS, AIME, vol. 244, septembre 1969, pages 283-287, New York, US; J.S. BROWNING: "Flotation of southeastern kyanite ore" * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103111364A (en) * | 2013-03-06 | 2013-05-22 | 合肥万泉非金属矿科技有限公司 | Technology of extracting quartz and feldspar from gangue |
CN103111364B (en) * | 2013-03-06 | 2014-12-17 | 合肥万泉非金属矿科技有限公司 | Technology of extracting quartz and feldspar from gangue |
Also Published As
Publication number | Publication date |
---|---|
ZA889630B (en) | 1990-03-28 |
FR2625115B1 (en) | 1990-10-19 |
FR2625115A1 (en) | 1989-06-30 |
DE3878440T2 (en) | 1993-09-16 |
EP0323323B1 (en) | 1993-02-10 |
AU609362B2 (en) | 1991-04-26 |
US4900431A (en) | 1990-02-13 |
AU2742488A (en) | 1989-06-29 |
DE3878440D1 (en) | 1993-03-25 |
CA1311864C (en) | 1992-12-22 |
ATE85537T1 (en) | 1993-02-15 |
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