WO2012079185A1 - Process for obtaining boron from natural or industrial and/or mineral brines that comprise boron, using an inorganic extractant for extracting the boron - Google Patents

Process for obtaining boron from natural or industrial and/or mineral brines that comprise boron, using an inorganic extractant for extracting the boron Download PDF

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Publication number
WO2012079185A1
WO2012079185A1 PCT/CL2011/000042 CL2011000042W WO2012079185A1 WO 2012079185 A1 WO2012079185 A1 WO 2012079185A1 CL 2011000042 W CL2011000042 W CL 2011000042W WO 2012079185 A1 WO2012079185 A1 WO 2012079185A1
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barium
boron
precipitate
solution
mineral
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PCT/CL2011/000042
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Spanish (es)
French (fr)
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Jorge Domingo Tapia Diaz
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Iholdi Minerales De Atacama Ltda
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B35/00—Boron; Compounds thereof
    • C01B35/02—Boron; Borides
    • C01B35/023—Boron

Definitions

  • the present invention relates to a Boron extraction process, by boron precipitation, with the use of a specific inorganic extractant that allows the boron to be separated directly from the concentrated brine, and without the need to use organic extractants, or water.
  • Boron is a semi-metallic element, which exhibits some properties of a metal and some of a non-metal element. In its elemental form it is a dark, amorphous and non-reactive solid. It is mainly used in the form of boron oxide (B 2 0 3) and boric acid (H3BO3), however not as elemental boron.
  • borax mineral which has been used mainly in the glass industry. Its main sources are the minerals that contain Boron, made up of a small number of borate (boron oxide) minerals, including Ulexite (NaCaB 5 09.8H 2 0), borax (Na 2 B 4 O 7 .10H 2 O), the colemanite (Ca 2 B 6 0n.5H 2 0), the hydroboracite, tincal and kernite (Na 2 B 4 0 6 (OH) 2 .3H 2 0). The main deposits of these minerals are in the United States, Turkey, Chile, Peru and Argentina. There are also certain boron silicate minerals in China and Russia, among others.
  • Boron compounds are applicable both in industry and at home. It is mainly used in the manufacture of glass, ceramics and enamels, including fiberglass for insulation. Boron compounds are also used for the manufacture of water softeners, soaps and detergents. Other uses of boron are found in agricultural chemicals, pest control agents, fire retardants, fireworks, medications, and various minor applications.
  • the process in synthesis consists in obtaining Li 2 C0 3 by pumping brine from the Salar to solar evaporation pools, where lithium is concentrated (approximately twenty-five times).
  • the concentrated product is sent for purification to a chemical plant ("La Negra" -Antofagasta).
  • the concentrated and pure product is treated with Na 2 C0 3 .
  • the extraction of the brine from the Salar is carried out with deep well pumps, placed in wells of about 30 thirty meters deep.
  • Said brines which generally have a content of about 0.2% by weight of lithium (measured by atomic absorption), are pumped to solar evaporation wells, where the objective is to concentrate the lithium in several stages until reaching a concentration of approximately 6% by weight of lithium.
  • the pools comprise layers of fine gravel and clays, and are kept covered with a waterproof PVC membrane and a second protective cover against the action of tillage machines and UV rays.
  • a waterproof PVC membrane and a second protective cover against the action of tillage machines and UV rays there are more than 15 pools of different sizes.
  • the process of obtaining lithium involves both the removal of discarding salts, for which in the first well a sulfate-rich brine is mixed with a calcium-rich brine, being eliminated at this stage the sulfate ion as a gypsum CaS0 4 » 2H 2 0, thus avoiding the precipitation of lithium in the form of sulfate, whereby the first discard salt is gypsum + halite: CaSCV2H 2 0 + NaCl. Then the fraction called silvinite (NaCl + KC1) precipitates,
  • lithium carnalite LiCl »MgCl 2 7H 2 0
  • the lithium contained in it is recovered by repulping the salt and washing with saturated MgCl 2 solution.
  • the final concentrated brine containing approximately 6% lithium; and about 2% of g and 0.7% of B is stored in a plastic coated pool, from where it is transported to Treatment Plants, in which the Boron is removed through an acid extraction process with solvent. Said process of separation of Boron or Boron compounds in this brine is initiated by adjusting the acidity of the brine with the addition of acid.
  • an organic extractant selected from the group consisting of 9-alkyl-salicylic-aldoxamine, ketoxime, beta-diketone, higher aliphatic alcohols, iso-octyl alcohol and naphtha, or a mixture of the above, preferably the mixture contains iso-octyl alcohol and naphtha in a 1: 1 ratio.
  • the brine that still contains Mg is subjected to the extraction of the latter as MgC0 3 and as Mg (OH) 2 .
  • the concentrated brine free of B and Mg is obtained, it is adjusted to a Li content of about 0.6%, and Na 2 CC> 3 hot (80-90 ° C) is added to the brine, precipitating in it Li 2 C0 3 , which is filtered and dried, obtaining it with a purity of Li 2 C0 3 of 99.5%.
  • the main objective of the present invention relates to the extraction of Boron from brines of natural or industrial origin or of minerals, where said Boron is in the form of Borate, Boric Acid Boron Hydroxide and Boric Oxide).
  • the production process of the present invention has a rapid and direct removal of boron, less polluting, which is achieved through the precipitation of boron compounds contained in brines of natural or industrial origin, or in aqueous mineral suspensions that contain boron, this precipitation is achieved by adding the novel inorganic extractant, composed of a barium salt, soluble in water, which is selected from the group consisting of Barium Chloride, Barium Oxide, Barium Hydroxide, Barium Fluoride, Sulfide Barium, Barium Sulfate, Di-Hydrated Barium Sulfate, Barium Sulfate, Barium Nitrate, Barium Carbonate, Barium Phosphate, Barium Bisulphite, Barium Hypochlorite, Barium Chlorate, Barium Peroxide, Barium Oxychloride, Barium Metabisulfite, Barium Chlorite, Barium Chlorate; where Barium Chloride can be anhydrous Barium Chloride and / or Barium Chlor
  • a salt of Barium Chloride (BaCl 2 ) is used directly on the solution / suspension comprising borates, thus precipitating the boron present immediately.
  • This process allows to obtain a precipitate of high purity borate, which can be subsequently processed to obtain boric acid with a high purity, and at the same time if it is required to continue with the extraction of the other elements present in the brine of the process already free of boron , if desired.
  • the sources of boron can be both brines and solutions / suspensions of minerals containing boron, with Ulexite and Borax standing out in the latter, both being minerals containing Boron.
  • Ulexite and Borax standing out in the latter, both being minerals containing Boron.
  • Borax is dissolved in water and sodium tetraborate dissociating into ions: NaCa ⁇ 5 0 9 ⁇ 8 H 2 0 + Ca +2 ⁇ Na + B 5 0 9 + 8 H 2 0
  • the tetraborate ion is hydrolyzed in water to hydroxyl ion and boric acid:
  • H2SO4 neutralizes the hydroxyl ion formed, shifting the balance to the right:
  • the tetraborate ion is hydrolyzed in water to hydroxyl ion and boric acid:
  • the object of the invention is to improve all the above-mentioned sections, modifying the current production process in obtaining Boric Acid, from natural or industrial brines, or from minerals such as Ulexite and Borax, since the present invention acts directly on the boron contained in the aforementioned sources immediately precipitating the borax in boric acid.
  • Figure 1 represents a scheme of the process of the invention, for obtaining boric acid, from brine.
  • Figure 2 represents a scheme of the process of the invention, for obtaining boric acid, from Ulexite.
  • Figure 3 represents a scheme of the process of the invention, for obtaining boric acid, from Borax.
  • the inorganic extractant of the present invention is composed of the soluble barium salts, indicated above, preferably Barium Chloride (BaCl 2 ).
  • This salt of Barium is what allows boron to precipitate, based on the chemical properties of Boron, which exhibits as an advantageous characteristic for the purpose of this invention, which is capable of reacting in a similar way to a metal, despite not Be a metal.
  • a water soluble barium salt preferably barium chloride
  • the inorganic extractant is applied in the process of the present invention by the following sequence of consecutive steps:
  • the inorganic extractant BaCl 2 is poured, directly on the brine of natural, mineral or industrial origin, or on a solution / suspension of mineral containing B, without the need to adjust the acidity of the boron source, initiating a selective precipitation of Barium borate, which is completed by mechanical agitation, according to the following reaction, in the case of extraction from: a) a natural or industrial brine:
  • the precipitate of Barium Borate obtained is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration is obtained from about 25% to 40% w / v, preferably from 28 to 35%, more preferably from 30% Barium Borate, which is mechanically stirred, said Barium Borate being hydrolyzed to form Boric acid, and allow the removal of barium in the form of a precipitate of barium sulfate, by adding sulfuric acid in a proportion between 1: 2 to 1: 3 of precipitate in solution: concentrated sulfuric acid (H 2 S0 4 c), where Boric acid is obtained with a purity of 99.5%, according to the following reaction: Ba (BO) 2 + 2H 2 0 + H 2 S0 + 2H 3 B0 3 .
  • the mineral must first be supplied in a particulate state, for which it is preferably ground to a size equal to or less than 15 mm. Then, this particulate material is suspended in water at 30 ° C until a 20% w / v solution of mineral is obtained, stirring mechanically for a period of 15 to 30 min, until reaching the total solution, then the inorganic extractant is added of BaCl 2 , in stoichiometric proportion, always under stirring, causing the following reaction:
  • the precipitate of the Boron salt obtained is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration of about 25% to 40% w / v, preferably 28 to 35%, more preferably 30% Barium Tetraborate, this solution is kept under stirring, said Tetraborate being hydrolyzed.
  • the mineral must first be supplied in a particulate state, for which it is preferably ground to a size equal to or less than 15 mm. Then, this particulate material is suspended in water at 30 ° C until a 20% w / v solution of mineral is obtained, stirring mechanically for a period of 15 to 30 min, until reaching the total solution, then the inorganic extractant is added of BaCl 2 , in stoichiometric proportion, always under stirring, causing the following reaction:
  • the precipitate of the Boron salt obtained is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration of about 25% to 40% w / v, preferably 28 to 35%, more preferably 30% of
  • Barium Pentaborate this solution is kept under stirring, said Barium Pentaborate being hydrolyzed to form Boric acid, and allowing the removal of barium as a precipitate of barium sulfate, by the addition of sulfuric acid in a ratio between 1: 2 at 1: 3 of precipitate in solution: concentrated sulfuric acid (H 2 S0 c), where Boric acid is obtained with a purity of 99.5%, according to the following reaction:
  • the inorganic BaCl 2 extractant used in the present invention can be added in the form of a previously prepared aqueous solution or be prepared in situ at the time of addition on the brine or mineral solution from which it is desired to extract the boron present.
  • This extractant allows a selective precipitation of the Boron component contained in the solution that is subjected to the extraction process, so even at very low concentrations it exhibits the effect of inducing the precipitation of borates, however, for a practical reproducibility effect it is preferred that the ratio of the extractant in the final reaction mixture is between 1 to 10% w / v, preferably between 2 to 7%, more preferably between 2.5 to 4.5%, much more preferably at a rate of 3% w / v.
  • the process of the present invention exhibits the following advantageous aspects, for example for its application in the production of Li from natural brines, with boron content, where boron separation is most effective, both in time and in the selective and non-polluting separation of it, in addition to exhibiting great economic advantages for the global process.
  • the process of the present invention involves the use of said Barium Chloride extractant, which allows the Boron to be extracted directly from natural or industrial brines and / or from minerals, independent of variables such as
  • the present invention relates to the production of boric acid from natural or industrial brines and / or minerals, by means of a new precipitation process of boron compounds.
  • the process of the present invention can be applied on a natural or industrial brine, independent of its geographical origin that has a composition that exhibits content of boron. This process is also applicable to aqueous solutions / suspensions of minerals, such as Ulexite and Borax.
  • the original volume of the treated brine or of the solution or suspension, from which the discard salts may optionally have been extracted, is introduced into a Reactor (about 1500 to 3000 L) in general at room temperature, in a range between 5 ° C and + 50 ° C.
  • the inorganic extractant is added, at a final concentration of about 3% w / v.
  • This mixture contained in said first reactor is stirred for a certain period of up to 1 hour, preferably between 15 and 45 minutes, more preferably between 15 and 30 minutes, and then allow a stand-by time of about 30 minutes, after which First, Boron precipitation will be obtained, which will be subsequently subjected to a purification and final extraction of boric acid, which allows obtaining this product with a purity of 99.5% and a water content of less than 0.5%.
  • a brine suitable for subjecting to the extraction process of the present invention is that of natural or industrial origin that complies with exhibiting any boron content, especially a content between 3000 to 10,000 ppm of B, preferably 7,000 to 9,000 ppm, more preferably one that contains 8000 ppm of Boron.
  • the Boron extraction process can be carried out in a brine of natural or industrial origin, as described below, through the specific examples representing the preferred embodiments of the invention. , it being understood that said examples are delivered oriented to limit the spectrum to its mere application, but that the invention can be carried out as different modalities through of the description given in this document and the routine knowledge of the average expert in the art.
  • the soluble barium salt, in the final product a mid-level expert in the art, will be prepared through its knowledge to detect and quantify the presence of said main element of the inorganic extractant, Barium, contained in the final product produced with the method for which protection is sought in the present application.
  • a brine is loaded into Reactor 1, according to the scheme of Figure 1, and the inorganic extractant or BaCl 2 is added directly, at room temperature, in a stoichiometric proportion, equivalent to a final 3% in volume of reaction; 2. It is mechanically stirred at the bottom of the reactor, for a period between 15 to 30 minutes;
  • the precipitate 1 obtained is filtered, through 5 mesh, to then lead it to reactor 2, with a volume capacity of about 2,000 liters, at room temperature,
  • the previous mixture shall be stirred with a mechanical stirrer, in its lower part, for a period between 15 to 30 minutes,
  • the pure Boric Acid obtained from the last stage is packaged, stored and distributed.
  • the pure Boric Acid obtained from the last stage of this example is packaged, stored and distributed.
  • 0E1 process of extraction of borates or boric acid from Borax ore can be carried out through the following stages:
  • the pure Boric Acid obtained from the last stage of this example is packaged, stored and distributed.
  • the present invention allows a transformation of the current way in which the industries related to industrial processes in which boron intervenes work, by directly extracting the boron from the brine or the minerals in suspension or solution, without making any dilution, nor the use of organic extractants, avoiding the generation of liquid industrial waste and avoiding the elimination of polluting final products.
  • Example 4 Boric Acid Extraction using Barium Phosphate from a natural or industrial brine.
  • the solid Boron salt contained in the precipitate is isolated by filtration through a sieve (for example 5 mesh), and then transferred this precipitate to a second reactor, at room temperature.
  • a second reactor water is added at a temperature of 80 to 98 ° C preferably between 82 to 95 ° C, more preferably at 92 ° C, to obtain a solution containing between 25 to 40%, preferably 28 to 35%, preferably 30% boric acid.
  • the above reaction mixture is maintained under mechanical stirring, in the lower part of the second reactor for about 15 to 30 minutes, then H 2 S0 4 c is added in a ratio of 1: 3, preferably 1: 2 of dissolved precipitate.
  • the mineral must first be supplied in a particulate state, for which it is preferably ground to a size equal to or less than 15 mm. Then this particulate material is suspended in water at 30 ° C until a 20% w / v solution of mineral is obtained, stirring mechanically for a period of 15 to 30 min, until reaching the total solution, then the inorganic extractant is added of Ba 3 (P0 4 ) 2 , in stoichiometric proportion, always under agitation, causing the following reaction:
  • the precipitate of the Boron salt obtained is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration of around 25% to 40% w / v, preferably 28 to 35%, more preferably 30% Barium Tetraborate, this solution is kept under stirring, said Barium Tetraborate being hydrolyzed to form Boric Acid, and allowing the barium to be removed in form of a precipitate of barium sulfate, by adding sulfuric acid in a proportion between 1: 2 to 1: 3 of precipitate in solution: concentrated sulfuric acid (H 2 S0 4 ) c where boric acid is obtained with a 99.5% purity, according to the following reaction: Bal3 ⁇ 4 (> 7 + 3H> S0 4 + 53 ⁇
  • the mineral must first be supplied in a particulate state, for which it is preferably ground to a size equal to or less than 15 mm. Then this particulate material is suspended in water at 30 ° C until a 20% w / v solution of mineral is obtained, stirring mechanically for a period of 15 to 30 min, until reaching the total solution, then the inorganic extractant is added of Ba3 (P0 4 ) 2 , eiiprc ordónestequiomerica, always under agitation, causing the following reaction:
  • the precipitate of the Boron salt obtained is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration of around 25% to 40% w / v, preferably 28 to 35%, more preferably 30% Barium Pentaborate, this solution is kept under stirring, said Barium Pentaborate being hydrolyzed to form Boric Acid, and allowing barium to be removed in form of a precipitate of barium sulfate, by adding sulfuric acid in a proportion between 1: 2 to 1: 3 of precipitate in solution: concentrated sulfuric acid H 2 S0 4 , where Boric acid is obtained with a purity of 99.5%, according to the following reaction:
  • the inorganic extractant Bas ⁇ PO ⁇ used in the present invention can be added in the form of a previously prepared aqueous solution or be prepared in situ at the time of the addition on the brine or mineral solution from which it is desired to extract the boron present.
  • This extractant allows a selective precipitation of the Boron component contained in the solution that is subjected to the extraction process, so even at very low concentrations it exhibits the effect of inducing the precipitation of borates, however, for a practical reproducibility effect it is preferred that the ratio of the extractant in the final reaction mixture is between 1 to 10% w / v, preferably between 2 to 7%, more preferably between 2.5 to 4.5%, much more preferably in a ratio of 3% p v.
  • a brine is loaded into a Reactor, and the inorganic extractant or BaF 2 is added directly, at room temperature, in a stoichiometric proportion, equivalent to a final 3% in the reaction volume; this reaction is maintained under mechanical stirring at the bottom of the reactor, for about 15 to 30 minutes; subsequently, the obtained mixture is allowed to stand for another period of about 15 to 30 minutes. From the previous rest a precipitate of Boron salt and a liquid solution are obtained. Subsequently, the solid salt containing Boron contained in the precipitate is isolated by filtration through a sieve (for example 5 mesh), and then transferred this precipitate to a second reactor, at room temperature.
  • a sieve for example 5 mesh
  • This second filtrate is dried, which comprises the boric acid, in a dryer, for example a continuous, at a temperature between about 100 to 150 ° C, to finally obtain dry boric acid, with a humidity degree of less than 0 , 5% water and with a concentration of 99.5%, according to the reaction indicated below. Pure Boric Acid obtained from the last stage is packaged and stored for later use and distribution.
  • the mineral must first be supplied in a particulate state, for which it is preferably ground to a size equal to or less than 15 mm. Then this particulate material is suspended in water at 30 ° C until a 20% w / v solution of mineral is obtained, stirring mechanically for a period of 15 to 30 min, until reaching the total solution, then the inorganic extractant is added of Ba F 2 , in stoichiometric proportion, always under agitation, causing the following reaction:
  • the precipitate of the Boron salt obtained is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration of around 25% to 40% w / v, preferably 28 to 35%, more preferably 30% Barium Tetraborate, this solution is kept under stirring, said Barium Tetraborate being hydrolyzed to form Boric Acid, and allowing the barium to be removed in form of a precipitate of barium sulfate, by the addition of sulfuric acid in a ratio between 1: 2 to 1: 3 of precipitate in solution: concentrated sulfuric acid (H2SO4), where Boric acid is obtained with a sump of 99.5 %, according to the following reaction:
  • the mineral must first be supplied in a particulate state, for which it is preferably ground to a size equal to or less than 15 mm. Then this particulate material is suspended in water at 30 ° C until a 20% w / v solution of mineral is obtained, stirring mechanically for a period of 15 to 30 min, until reaching the total solution, then the inorganic extractant is added of BaF 2 , in stoichiometric proportion, always under agitation, causing the following reaction:
  • the precipitate of the Boron salt obtained is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration of around 25% to 40% w / v, preferably 28 to 35%, more preferably 30% Barium Pentaborate, this solution is kept under stirring, said Barium Pentaborate being hydrolyzed to form Boric Acid, and allowing barium to be removed in form of a precipitate of barium sulfate, by adding sulfuric acid in a proportion between 1: 2 to 1: 3 of precipitate in solution: concentrated sulfuric acid H 2 S0 4 , where Boric acid is obtained with a purity of 99.5%, according to the following reaction:
  • the inorganic extractant BaF 2 used in the present invention can be added in the form of a previously prepared aqueous solution or be prepared in situ at the time of the addition on the brine or mineral solution from which it is desired to extract the boron present.
  • This extractant allows a selective precipitation of the Boron component contained in the solution that is subjected to the extraction process, so even at very low concentrations it exhibits the effect of inducing the precipitation of borates, however, for a practical reproducibility effect it is preferred that the ratio of the extractant in the final reaction mixture is between 1 to 10% w / v, preferably between 2 to 7%, more preferably between 2.5 to 4.5%, much more preferably at a rate of 3% w / v.
  • a brine is loaded into a Reactor, and the inorganic extractant or BaO is added directly, at room temperature, in a stoichiometric proportion, equivalent to a final 3% in the reaction volume; this reaction is maintained under mechanical stirring at the bottom of the reactor, for about 15 to 30 minutes; subsequently, the obtained mixture is allowed to stand for another period of about 15 to 30 minutes. From the previous rest a precipitate of Boron salt and a liquid solution are obtained. Subsequently, the solid salt containing Boron contained in the precipitate is isolated by filtration through a sieve (for example 5 mesh), and then transferred this precipitate to a second reactor, at room temperature.
  • a sieve for example 5 mesh
  • This second filtrate is dried, which comprises the boric acid, in a dryer, for example a continuous, at a temperature between about 100 to 150 ° C, to finally obtain dry boric acid, with a humidity degree of less than 0 ,5% of water and with a concentration of 99.5%, according to the reaction indicated below. Pure Boric Acid obtained from the last stage is packaged and stored for later use and distribution.
  • the mineral must first be supplied in a particulate state, for which it is preferably ground to a size equal to or less than 15 mm. Immediately this particulate material is suspended in water at 30 ° C until a 20% w / v solution of mineral is obtained, stirring mechanically for a period of 15 to 30 min, until reaching the total solution, then the inorganic extractant is added of BaO, in stoichiometric proportion, always under agitation, causing the following reaction:
  • the precipitate of the Boron salt obtained is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration of about 25% to 40% w / v, preferably 28 to 35%, more preferably 30% of Barium Tetraborate, this solution is kept under stirring, said Barium Tetraborate being hydrolyzed to form Boric acid, and allowing the removal of barium in the form of a precipitate of barium sulfate, by the addition of sulfuric acid in a proportion between 1: 2 a 1: 3 precipitate in solution: concentrated sulfuric acid (H 2 S0 4 c), where Boric acid is obtained with a purity of 99.5%, according to the following reaction:
  • the mineral must first be supplied in a particulate state, for which it is preferably ground to a size equal to or less than 15 mm. Immediately this particulate material is suspended in water at 30 ° C until a 20% w / v solution of mineral is obtained, stirring mechanically for a period of 15 to 30 min, until reaching the total solution, then the inorganic extractant is added of BaO, in stoichiometric proportion, always under agitation, causing the following reaction:
  • the precipitate of the Boron salt obtained is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration of about 25% to 40% w / v, preferably 28 to 35%, more preferably 30% Barium Pentaborate, this solution is kept under stirring, said Barium Pentaborate being hydrolyzed to form Boric Acid, and allowing barium to be removed as a precipitate of barium sulfate, by the addition of sulfuric acid in a proportion between 1: 2 to 1: 3 of precipitate in solution: concentrated sulfuric acid (H 2 S0 4 c), where Boric acid is obtained with a purity 99.5%, according to the following reaction: .0.0 Ba 3 (B 5 0 9 ) 2 + 12H 2 0 + 3H 2 S0 4 ⁇ 3BaS0 4 + 10H 3 BO 3
  • the inorganic BaO extractant used in the present invention can be added in the form of a previously prepared aqueous solution or be prepared in situ at the time of the addition on the brine or mineral solution from which it is desired to extract the boron present.
  • This extractant allows a selective precipitation of the Boron component contained in the solution that is subjected to the extraction process, so even at very low concentrations it exhibits the effect of inducing the precipitation of borates, however, for a practical reproducibility effect it is preferred that the ratio of the extractant in the final reaction mixture is between 1 to 10% w / v, preferably between 2 to 7%, more preferably between 2.5 to 4.5%, much more preferably at a rate of 3% w / v.
  • a brine is loaded into a Reactor, and the inorganic extractant or Ba (N0 3 ) 2 is added directly, at room temperature, in a stoichiometric proportion, equivalent to a final 3% in the reaction volume; this reaction is maintained under mechanical stirring at the bottom of the reactor, for about 15 to 30 minutes; subsequently, the obtained mixture is allowed to stand for another period of about 15 to 30 minutes. From the previous rest a precipitate of Boron salt and a liquid solution are obtained. Subsequently, the solid salt containing Boron contained in the precipitate is isolated by filtration through a sieve (for example 5 mesh), and then transferred this precipitate to a second reactor, at room temperature.
  • a sieve for example 5 mesh
  • This second filtrate is dried, which comprises the boric acid, in a dryer, for example a continuous, at a temperature between about 100 to 150 ° C, to finally obtain dry boric acid, with a humidity degree of less than 0 , 5% water and with a concentration of 99.5%, according to the reaction indicated below.
  • Pure Boric Acid obtained from the last stage is packaged and stored for later use and distribution.
  • the mineral must first be supplied in a particulate state, for which it is preferably ground to a size equal to or less than 15 mm. Then this particulate material is suspended in water at 30 ° C until a 20% w / v solution of mineral is obtained, stirring mechanically for a period of 15 to 30 min, until reaching the total solution, then the inorganic extractant is added of Ba (N0 3 ) 2 , in stoichiometric proportion, always under agitation, causing the following reaction:
  • the precipitate of the Boron salt obtained is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration of around 25% to 40% w / v, preferably 28 to 35%, more preferably 30% Barium Tetraborate, this solution is kept under stirring, said Barium Tetraborate being hydrolyzed to form Boric Acid, and allowing the barium to be removed in form of a precipitate of barium sulfate, by adding sulfuric acid in a proportion between 1: 2 to 1: 3 of precipitate in solution: concentrated sulfuric acid (H 2 S0 4 ), where Boric acid is obtained with a 99.5% purity, according to the following reaction: BaRfh + 511 ⁇ 40 + ⁇ 0 4 ⁇ BaS
  • the mineral must first be supplied in a particulate state, for which it is preferably ground to a size equal to or less than 15 mm. Then this particulate material is suspended in water at 30 ° C until a 20% w / v solution of mineral is obtained, stirring mechanically for a period of 15 to 30 min, until reaching the total solution, then the inorganic extractant is added of Ba (N0 3 ) 2 , in stoichiometric proportion, always under agitation, causing the following reaction:
  • the precipitate of the Boron salt obtained is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration of around 25% to 40% w / v, preferably 28 to 35%, more preferably 30% Barium Pentaborate, this solution is kept under stirring, said Barium Pentaborate being hydrolyzed to form Boric Acid, and allowing barium to be removed in form of a precipitate of Barium sulfate, by adding sulfuric acid in a proportion between 1: 2 and 1: 3 of precipitate in solution: concentrated sulfuric acid (H2S04C), where Boric acid is obtained with a purity of 99.5%, according to The following reaction:
  • the inorganic extractant Ba (N0 3 ) 2 used in the present invention can be added in the form of a previously prepared aqueous solution or be prepared in situ at the time of addition on the brine or mineral solution from which it is desired to extract the Boron present.
  • This extractant allows a selective precipitation of the Boron component contained in the solution that is subjected to the extraction process, so even at very low concentrations it exhibits the effect of inducing the precipitation of borates, however, for a practical reproducibility effect it is preferred that the ratio of the extractant in the final reaction mixture is between 1 to 10% w / v, preferably between 2 to 7%, more preferably between 2.5 to 4.5%, much more preferably at a rate of 3% w / v.

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Abstract

The invention relates to a process for extracting boron from brines of natural or industrial origin, or boron contained in a boron-containing mineral. According to the invention, the process is carried out without the need for acidity adjustment and without solvents and the boron content is precipitated using an inorganic extractant.

Description

PROCESO DE OBTENCIÓN DE BORO A PARTIR DE SALMUERAS NATURALES O INDUSTRIALES Y/O MINERALES QUE COMPRENDEN BORO, UTILIZANDO UN EXTRACTANTE INORGÁNICO PARA EXTRAER EL BORO.  PROCESS OF OBTAINING BORO FROM NATURAL OR INDUSTRIAL AND / OR MINERAL SALMUERAS THAT INCLUDE BORO, USING AN INORGANIC EXTRACTANT TO REMOVE THE BORO.
MEMORIA DESCRIPTIVA DESCRIPTIVE MEMORY
La presente invención se refiere a un procedimiento de extracción de Boro, mediante precipitación de boro, con el uso de un extractante inorgánico específico que permite separar el boro directamente de la salmuera concentrada, y sin necesidad de tener que utilizar extractantes orgánicos, ni agua.  The present invention relates to a Boron extraction process, by boron precipitation, with the use of a specific inorganic extractant that allows the boron to be separated directly from the concentrated brine, and without the need to use organic extractants, or water.
Igualmente aplicable para su obtención a partir de minerales como Ulexita y Bórax, en forma de soluciones que comprenden alrededor de 20% de dichos minerales, respectivamente. ANTECEDENTES DE LA INVENCION  Equally applicable for obtaining from minerals such as Ulexite and Borax, in the form of solutions comprising about 20% of said minerals, respectively. BACKGROUND OF THE INVENTION
Si bien el Boro se encuentra presente tanto en minerales, salmueras naturales o de origen industrial, durante décadas se han desarrollado diversos métodos para extraerlo, y en la actualidad solo dos procesos de obtención son económicamente factibles; de minerales y salmueras.  Although Boron is present in both minerals, natural or industrial brines, for decades various methods have been developed to extract it, and currently only two production processes are economically feasible; of minerals and brines.
El boro es un elemento semi-metálico, que exhibe algunas propiedades de un metal y algunas de un elemento no metal. En su forma elemental es un sólido oscuro, amorfo y no reactivo. Se utiliza principalmente bajo la forma de óxido de boro (B203) y de ácido bórico (H3BO3), sin embargo no como Boro elemental. Boron is a semi-metallic element, which exhibits some properties of a metal and some of a non-metal element. In its elemental form it is a dark, amorphous and non-reactive solid. It is mainly used in the form of boron oxide (B 2 0 3) and boric acid (H3BO3), however not as elemental boron.
Su nombre proviene del mineral bórax, el cual se ha utilizado en la industria del vidrio principalmente. Sus principales fuentes son los minerales que contienen Boro, conformados por un pequeño número de minerales de borato (óxido de boro), incluyendo a la Ulexita (NaCaB509.8H20), el bórax (Na2B4O7.10H2O), la colemanita (Ca2B60n.5H20), la hidroboracita, tincal y kernita (Na2B406(OH)2.3H20). Los principales depósitos de estos minerales se encuentran en Estados Unidos, Turquía, Chile, Bolivia y Argentina. Existen además ciertos minerales de boro silicato en China y Rusia, entre otros. Its name comes from the borax mineral, which has been used mainly in the glass industry. Its main sources are the minerals that contain Boron, made up of a small number of borate (boron oxide) minerals, including Ulexite (NaCaB 5 09.8H 2 0), borax (Na 2 B 4 O 7 .10H 2 O), the colemanite (Ca 2 B 6 0n.5H 2 0), the hydroboracite, tincal and kernite (Na 2 B 4 0 6 (OH) 2 .3H 2 0). The main deposits of these minerals are in the United States, Turkey, Chile, Bolivia and Argentina. There are also certain boron silicate minerals in China and Russia, among others.
El uso de los compuestos de Boro tiene aplicación tanto en la industria como en el hogar. Se utiliza principalmente en la fabricación de vidrio, cerámicas y esmaltes, incluyendo a la fibra de vidrio para aislación. También se utilizan los compuestos de boro para la fabricación de ablandadores de agua, jabones y detergentes. Otros usos del boro se encuentran en los productos químicos agrícolas, agentes de control de plagas, retardadores de fuego, fuegos artificiales, medicamentos, y diversas aplicaciones menores.  The use of Boron compounds is applicable both in industry and at home. It is mainly used in the manufacture of glass, ceramics and enamels, including fiberglass for insulation. Boron compounds are also used for the manufacture of water softeners, soaps and detergents. Other uses of boron are found in agricultural chemicals, pest control agents, fire retardants, fireworks, medications, and various minor applications.
La extracción de Boro cobra importancia en procesos de separación y purificación de diversos elementos provenientes de minerales y/o salmueras, en los cuales este componente se encuentra contenido junto a otros elementos de interés, donde por lo general es necesario primero extraer el Boro para proceder a la separación de los restantes elementos, cobrando importancia por ejemplo en la producción de carbonato de litio proveniente de minerales, como por ejemplo espodumeno. La solicitud CN101712481 describe un método para preparar carbonato de litio de elevada pureza y otros subproductos a partir de salmuera proveniente de salar que consiste en primero separar el potasio y sodio de la salmuera mediante exposición de la sal a un campo de sal, para luego separar el boro mediante acidificación, y continuar con la posterior separación de magnesio y calcio, preparar cloruro de litio, para finalmente obtener carbonato de litio. Este documento describe un método para purificar iones entre los cuales está comprendido el boro entre otros. La patente US 4261960 (A) describe un proceso de extracción, en el cual el boro, así como las impurezas del magnesio y del sulfato, son separadas o reducidas en una salmuera que contiene Litio. Boron extraction becomes important in processes of separation and purification of various elements from minerals and / or brines, in which this component is contained along with other elements of interest, where it is usually necessary first to extract the Boron to proceed to the separation of the remaining elements, gaining importance for example in the production of lithium carbonate from minerals, such as spodumene. Application CN101712481 describes a method for preparing high purity lithium carbonate and other by-products from brine from salt which consists in first separating potassium and sodium from brine by exposing the salt to a salt field, then separating Boron by acidification, and continue with the subsequent separation of magnesium and calcium, prepare lithium chloride, to finally obtain lithium carbonate. This document describes a method to purify ions among which boron is included among others. US 4261960 (A) describes an extraction process, in which the boron, as well as the impurities of magnesium and sulfate, are separated or reduced in a brine containing Lithium.
La patente US 6.207.126 de Chemetall Foote Corporation, describe un proceso de obtención de Li a partir de salmueras en él se menciona el uso de cloruro de Bario como precipitante para retirar el sulfato, precipitándolo como sulfato de bario, siendo esta una reacción característica. En dicho proceso se retira el Mg de la salmuera como una sal doble con un exceso de soda (CaO), separando los lodos de Mg y Ca mediante filtración, con etapas de remoción de Na y de dilución de la salmuera a la cual finalmente se le adiciona un precipitante de Ca y cloruro de bario para remover el sulfato, lo cual finalmente permite obtener una salmuera limpia para la posterior recuperación del cloruro de litio.  US Patent 6,207,126 of Chemetall Foote Corporation, describes a process of obtaining Li from brines in it mentioning the use of barium chloride as a precipitant to remove sulfate, precipitating it as barium sulfate, this being a characteristic reaction . In this process, the Mg is removed from the brine as a double salt with an excess of soda (CaO), separating the sludge from Mg and Ca by filtration, with Na removal and dilution steps of the brine at which it is finally a precipitate of Ca and barium chloride is added to remove the sulfate, which finally allows a clean brine to be obtained for the subsequent recovery of lithium chloride.
También es conocido en el estado del arte que la Sociedad Chilena del Litio (SCL), lleva a cabo un proceso de producción de carbonato de litio, a partir de salmuera en el cual es necesario retirar el boro en una etapa previa. Este proceso utilizado por la Sociedad Chilena del Litio (SCL), se aplica en la extracción de litio proveniente de salmueras naturales que comprenden boro, las cuales exhiben una elevada razón Li/Mg (Salar de Atacama) debido a la concentración de Li, lo que hace que el procedimiento requiera de una etapa previa de evaporación solar para concentrar las sales de Mg y separarlas por concentración. El proceso en síntesis consiste en obtener Li2C03 por bombeo de salmueras del Salar a pozas de evaporación solar, donde se concentra el litio (aproximadamente veinticinco veces). El producto concentrado se envía a purificación a una planta química ("La Negra"-Antofagasta). El producto concentrado y puro se trata con Na2C03. La extracción de las salmueras del Salar, se realiza con bombas de pozo profundo, colocadas en pozos de alrededor de 30 treinta metros de profundidad. Dichas salmueras, que en general presentan un contenido de alrededor de 0,2 % en peso de litio (medido por absorción atómica), son bombeadas a pozos de evaporación solar, donde el objetivo es concentrar el litio en varias etapas hasta alcanzar una concentración de aproximadamente 6% en peso de litio. Esta operación de concentración por evaporación es lenta, demora alrededor de un año. Las pozas comprenden capas de grava fina y arcillas, y se mantienen cubiertas con una membrana impermeable de PVC y una segunda cubierta de protección frente a la acción de las máquinas de laboreo y de los rayos UV. En la actualidad existen más de 15 pozas de diferentes tamaños. El proceso de obtención de litio, que requiere de la remoción de boro, involucra a la vez la remoción de sales de descarte, para lo cual en la primera poza se mezcla una salmuera rica en sulfato con otra rica en calcio, eliminándose en esta etapa el ión sulfato como yeso CaS04 »2H20, evitando de este modo la precipitación del litio en forma de sulfato, por lo cual la primera sal de descarte es yeso + halita: CaSCV2H20 + NaCl. Luego precipita la fracción denominada: silvinita (NaCl + KC1), It is also known in the state of the art that the Chilean Society of Lithium (SCL), carries out a process of production of lithium carbonate, from brine in which it is necessary to remove the boron at a previous stage. This process used by the Chilean Society of Lithium (SCL), is applied in the extraction of lithium from natural brines comprising boron, which exhibit a high ratio Li / Mg (Salar de Atacama) due to the concentration of Li, which makes the process require a previous stage of solar evaporation to concentrate the Mg salts and separate them by concentration. The process in synthesis consists in obtaining Li 2 C0 3 by pumping brine from the Salar to solar evaporation pools, where lithium is concentrated (approximately twenty-five times). The concentrated product is sent for purification to a chemical plant ("La Negra" -Antofagasta). The concentrated and pure product is treated with Na 2 C0 3 . The extraction of the brine from the Salar, is carried out with deep well pumps, placed in wells of about 30 thirty meters deep. Said brines, which generally have a content of about 0.2% by weight of lithium (measured by atomic absorption), are pumped to solar evaporation wells, where the objective is to concentrate the lithium in several stages until reaching a concentration of approximately 6% by weight of lithium. This evaporation concentration operation is slow, it takes about a year. The pools comprise layers of fine gravel and clays, and are kept covered with a waterproof PVC membrane and a second protective cover against the action of tillage machines and UV rays. Currently there are more than 15 pools of different sizes. The process of obtaining lithium, which requires the removal of boron, involves both the removal of discarding salts, for which in the first well a sulfate-rich brine is mixed with a calcium-rich brine, being eliminated at this stage the sulfate ion as a gypsum CaS0 4 » 2H 2 0, thus avoiding the precipitation of lithium in the form of sulfate, whereby the first discard salt is gypsum + halite: CaSCV2H 2 0 + NaCl. Then the fraction called silvinite (NaCl + KC1) precipitates,
carnalita (KCl«MgCl2 » 6H20), y carnalite (KCl " MgCl 2 " 6H 2 0), and
Bischofita (MgCl2 »6H20). Bischophyte (MgCl 2 » 6H 2 0).
Además precipita, carnalita de litio (LiCl»MgCl2 7H20), y se recupera el litio contenido en ella mediante repulpaje de la sal y lavado con solución saturada de MgCl2. La bischofita, (MgCl2*6H20) no disuelta se retira mediante centrifugación. It also precipitates, lithium carnalite (LiCl »MgCl 2 7H 2 0), and the lithium contained in it is recovered by repulping the salt and washing with saturated MgCl 2 solution. Bischophyte, (undissolved MgCl 2 * 6H 2 0) is removed by centrifugation.
Finalmente la salmuera concentrada final que contiene aproximadamente un 6% de litio; y alrededor de 2% de g y 0,7% de B se almacena en una poza revestida con plástico, desde donde se transporta a Plantas de Tratamiento, en ellas se retira el Boro a través de un proceso de extracción ácida con solvente. Dicho proceso de separación de Boro o de compuestos de Boro en esta salmuera, se inicia mediante el ajuste de la acidez de la salmuera con adición de ácido sulfúrico hasta alcanzar un pH de 2, para luego extraer mediante el uso de un extractante orgánico, seleccionado del grupo formado por 9-alquil-salicil-aldoxamina, cetoxima, beta- dicetona, alcoholes alifáticos superiores, alcohol iso-octílico y nafta, o una mezcla de los anteriores, preferentemente la mezcla contiene alcohol iso-octílico y nafta en una proporción 1 :1. Posteriormente, la salmuera que aun contiene Mg, se somete a la extracción de este último como MgC03 y como Mg (OH)2. Una vez obtenida la salmuera concentrada libre de B y Mg, se procede a ajustar a un contenido de Li de alrededor de 0,6%, y se agrega Na2CC>3 en caliente (80- 90°C) a la salmuera, precipitando en ella Li2C03, el cual es filtrado y secado, obteniéndolo con una pureza de Li2C03 de 99,5%. Finally, the final concentrated brine containing approximately 6% lithium; and about 2% of g and 0.7% of B is stored in a plastic coated pool, from where it is transported to Treatment Plants, in which the Boron is removed through an acid extraction process with solvent. Said process of separation of Boron or Boron compounds in this brine is initiated by adjusting the acidity of the brine with the addition of acid. sulfuric acid until a pH of 2 is reached, and then extracted by using an organic extractant, selected from the group consisting of 9-alkyl-salicylic-aldoxamine, ketoxime, beta-diketone, higher aliphatic alcohols, iso-octyl alcohol and naphtha, or a mixture of the above, preferably the mixture contains iso-octyl alcohol and naphtha in a 1: 1 ratio. Subsequently, the brine that still contains Mg is subjected to the extraction of the latter as MgC0 3 and as Mg (OH) 2 . Once the concentrated brine free of B and Mg is obtained, it is adjusted to a Li content of about 0.6%, and Na 2 CC> 3 hot (80-90 ° C) is added to the brine, precipitating in it Li 2 C0 3 , which is filtered and dried, obtaining it with a purity of Li 2 C0 3 of 99.5%.
DESCRIPCION DE LA INVENCION DESCRIPTION OF THE INVENTION
El objetivo principal de la presente invención se relaciona con la extracción de Boro a partir de salmueras de origen natural o industrial o bien de minerales, donde dicho Boro se encuentra en la forma de Borato, Acido Bórico Hidróxido de boro y óxido Bórico). The main objective of the present invention relates to the extraction of Boron from brines of natural or industrial origin or of minerals, where said Boron is in the form of Borate, Boric Acid Boron Hydroxide and Boric Oxide).
En la actualidad, la industria de obtención de boro a partir de las mismas fuentes indicadas anteriormente, utiliza extractantes orgánicos junto a grandes volúmenes de agua, lo cual además de ser costoso representa un proceso poco amigable con el medioambiente. At present, the industry of obtaining boron from the same sources indicated above, uses organic extractants along with large volumes of water, which in addition to being expensive represents an unfriendly process with the environment.
El proceso productivo de la presente invención presenta una rápida y directa remoción de boro, menos contaminante, lo cual se logra a través de la precipitación de los compuestos de boro contenidos en salmueras de origen natural o industrial, o bien en suspensiones acuosas de minerales que contienen boro, dicha precipitación se logra al adicionar el novedoso extractante inorgánico, compuesto por una sal de Bario, soluble en agua, la cual se selecciona del grupo formado por Cloruro de Bario, Oxido de Bario, Hidróxido de Bario, Fluoruro de Bario, Sulfuro de Bario, Sulfato de Bario, Sulfato de Bario Di-hidratado, Sulfito de Bario, Nitrato de Bario, Carbonato de Bario, Fosfato de Bario, Bisulfito de Bario, Hipoclorito de Bario, Clorato de Bario, Peróxido de Bario, Oxicloruro de Bario, Metabisulfito de Bario, Clorito de Bario, Clorato de Bario; donde el Cloruro de Bario puede ser Cloruro de Bario anhidro y/o Cloruro de Bario hexahidratado. De preferencia se utiliza una sal de Cloruro de Bario (BaCl2) directamente sobre la solución/suspensión que comprende boratos, precipitando de este modo el boro presente de forma inmediata. Este proceso permite obtener un precipitado de borato de alta pureza, que puede ser posteriormente procesado para obtener ácido bórico con una elevada pureza, y a la vez si se requiere continuar con la extracción de los otros elementos presentes en la salmuera del proceso ya libre de boro, si se desea. The production process of the present invention has a rapid and direct removal of boron, less polluting, which is achieved through the precipitation of boron compounds contained in brines of natural or industrial origin, or in aqueous mineral suspensions that contain boron, this precipitation is achieved by adding the novel inorganic extractant, composed of a barium salt, soluble in water, which is selected from the group consisting of Barium Chloride, Barium Oxide, Barium Hydroxide, Barium Fluoride, Sulfide Barium, Barium Sulfate, Di-Hydrated Barium Sulfate, Barium Sulfate, Barium Nitrate, Barium Carbonate, Barium Phosphate, Barium Bisulphite, Barium Hypochlorite, Barium Chlorate, Barium Peroxide, Barium Oxychloride, Barium Metabisulfite, Barium Chlorite, Barium Chlorate; where Barium Chloride can be anhydrous Barium Chloride and / or Barium Chloride hexahydrate. Preferably, a salt of Barium Chloride (BaCl 2 ) is used directly on the solution / suspension comprising borates, thus precipitating the boron present immediately. This process allows to obtain a precipitate of high purity borate, which can be subsequently processed to obtain boric acid with a high purity, and at the same time if it is required to continue with the extraction of the other elements present in the brine of the process already free of boron , if desired.
En el estado del arte, específicamente en el proceso mencionado anteriormente, se pueden apreciar las siguientes características:  In the state of the art, specifically in the process mentioned above, the following characteristics can be appreciated:
1. - el proceso requiere de extractantes orgánicos para separar el boro de la salmuera, en una relación elevada entre salmuera y extractante orgánico, en general la relación es de 1 : 1 en volumen,  1. - the process requires organic extractants to separate the boron from the brine, in a high ratio between brine and organic extractant, in general the ratio is 1: 1 by volume,
2. - los extractantes orgánicos utilizados en esta industria, poseen un bajo punto de inflamación y una elevada volatilidad, representando altos riesgos en la realización del proceso, tanto para el personal como para las maquinarias,  2. - The organic extractants used in this industry, have a low flash point and high volatility, representing high risks in the process, both for personnel and machinery,
3. - El proceso consume un importante volumen de agua, equivalente a una relación de alrededor de 1 L de agua por cada 10 g de B, representando alrededor de 80.000 litros por cada tonelada de Boro,  3. - The process consumes a significant volume of water, equivalent to a ratio of about 1 L of water for every 10 g of B, representing around 80,000 liters per ton of Boron,
4.- El agua utilizada en el proceso de extracción del boro, resulta siendo agua contaminada con extractantes orgánicos, más bien conocida como un residuo industrial liquido 4.- The water used in the boron extraction process turns out to be water contaminated with organic extractants, rather known as a liquid industrial waste
(riles), por lo cual se requiere de su debido tratamiento, para evitar provocar contaminación a napas de agua en dichas zonas desérticas. (riles), which requires its proper treatment, to avoid causing contamination to water sheets in these desert areas.
5.- La ubicación geográfica de este tipo de yacimientos se encuentra en zonas áridas y desérticas, zonas en las cuales es sabido que el recurso del agua es escaso, 6. - El uso de pozas de evaporación solar, en grandes extensiones de terreno para facilitar la evaporación, representa un evidente riesgo de filtración, y por ende una constante amenaza de contaminación ambiental, 5.- The geographical location of this type of deposits is found in arid and desert areas, areas in which it is known that water resources are scarce, 6. - The use of solar evaporation ponds, in large areas of land to facilitate evaporation, represents an obvious risk of filtration, and therefore a constant threat of environmental pollution,
7. - La salmuera obtenida una vez que se han eliminado las sales de descarte debe ser transportada a Plantas del tratamiento final, lo que redunda en aumentos de costo y tiempos de realización del proceso,  7. - The brine obtained once the discarding salts have been eliminated must be transported to the plants of the final treatment, which results in cost increases and process completion times,
8. - El uso de grandes volúmenes de agua, disminuye la concentración final de los innumerables cationes y aniones que normalmente están presentes en la salmuera, en forma de moléculas hidratadas, haciendo que se pierda el interés comercial por dichas sales debido a la baja concentración final,  8. - The use of large volumes of water decreases the final concentration of the innumerable cations and anions that are normally present in the brine, in the form of hydrated molecules, causing commercial interest in these salts to be lost due to the low concentration final,
9. - Las sales antes mencionadas se transforman en desechos, lo cual requiere de una eliminación adecuada para no afectar el Medio Ambiente.  9. - The aforementioned salts are transformed into waste, which requires adequate disposal so as not to affect the environment.
En vista de las desventajosas características antes mencionadas, existe la necesidad de mejorar varios de los aspectos anteriormente indicados, modificando el actual proceso productivo de modo de considerar una remoción de boro más directa, menos contaminante y más ecológica, lo cual se logra a través del proceso de la presente invención, que permite actuar directamente sobre el boro presente en las salmueras o en la solución/suspensión que se utilice como materia prima, precipitando de forma inmediata el boro presente, mediante la adición de la sal de Bario soluble, preferentemente cloruro de bario, y dejando en solución libres aquellos elementos de interés para su posterior extracción, como por ejemplo el litio en el caso del proceso realizado por SCL.In view of the aforementioned disadvantageous characteristics, there is a need to improve several of the aforementioned aspects, modifying the current production process in order to consider a more direct, less polluting and more ecological boron removal, which is achieved through the process of the present invention, which allows to act directly on the boron present in the brines or in the solution / suspension that is used as raw material, immediately precipitating the boron present, by adding the soluble barium salt, preferably chloride of barium, and leaving in solution free those elements of interest for its subsequent extraction, such as lithium in the case of the process carried out by SCL.
Tal como se indicó previamente las fuentes de boro pueden ser tanto salmueras, como soluciones/suspensiones de minerales que contienen boro, destacándose dentro de estos últimos la Ulexita y el Bórax, ambos siendo minerales que contienen Boro. Específicamente en el caso de aplicar el proceso del estado del arte sobre los minerales ULEXITA ( aCaB509*8H20) y BORAX (Na2B4O7 »10H2O), se hacen evidentes las siguientes características: As previously indicated, the sources of boron can be both brines and solutions / suspensions of minerals containing boron, with Ulexite and Borax standing out in the latter, both being minerals containing Boron. Specifically in the case of applying the state of the art process on the minerals ULEXITA (aCaB 5 0 9 * 8H 2 0) and BORAX (Na 2 B 4 O 7 » 10H 2 O), the following characteristics become evident:
1. - El mineral previamente molido de Ulexita o de Bórax, se debe verter en las pozas artificiales,  1. - The previously ground ore of Ulexite or Borax must be poured into artificial pools,
2. - Como los boratos presentan una baja solubilidad (alrededor de un 3%) se necesitan pozas artificiales con una gran extensión, debido a los importantes volúmenes de agua requeridos,  2. - As borates have a low solubility (around 3%), artificial ponds with a large extension are needed, due to the large volumes of water required,
3. - Se utilizan pozas artificiales de poca profundidad, para mejorar la evaporación en ellas, lo cual hace que la extensión de terreno requerida sea de grandes dimensiones,  3. - Shallow artificial pools are used to improve evaporation in them, which makes the required area of land large.
4. - La existencia de pozas, representa un potencial riesgo de contaminación medioambiental por la presencia de compuestos tóxicos, debido a la alta probabilidad que ocurra una filtración hacia napas subterráneas,  4. - The existence of ponds represents a potential risk of environmental contamination due to the presence of toxic compounds, due to the high probability that a filtration will occur towards underground layers,
5. - La ubicación geográfica de estos minerales, hace que la gran cantidad de agua necesaria, sea un costo adicional para lograr la extracción y cristalización, poco viable en zonas desérticas,  5. - The geographical location of these minerals, makes the large amount of water necessary, an additional cost to achieve extraction and crystallization, unfeasible in desert areas,
6. - Se requiere de una gran cantidad de Acido sulfúrico para acidificar estas soluciones, 6. - A large amount of sulfuric acid is required to acidify these solutions,
7. - Se genera una gran cantidad de residuos industriales sólidos (sales de descarte), que permanecen dentro de las pozas artificiales, representando nuevamente un grave problema para el Medio Ambiente, 7. - A large amount of solid industrial waste (discarding salts) is generated, which remain inside artificial pools, again representing a serious problem for the Environment,
9.- Una vez re-cristalizado el ácido bórico en dichas pozas se cosecha, se envasa y transporta a una planta de tratamiento posterior, lo cual hace que se vuelva a precisar de grandes cantidades de agua a una temperatura superior a 90°C, así como del uso de acetona o éter etílico (solventes), a fin de obtener acido bórico de alta pureza. Por lo anterior, además se puede resumir que en el proceso de obtención de Acido bórico del arte previo a partir del Mineral Ulexita, se encuentran implícitas las siguientes reacciones: 9.- Once the boric acid in these pools is re-crystallized, it is harvested, packaged and transported to a subsequent treatment plant, which means that large amounts of water are required again at a temperature higher than 90 ° C, as well as the use of acetone or ethyl ether (solvents), in order to obtain boric acid of high purity. Therefore, it can also be summarized that in the process of obtaining Boric Acid from the prior art from Ulexite Mineral, the following reactions are implicit:
El Bórax se disuelve en el agua disociándose en iones sodio y tetraborato: NaCa Β509·8 H20 ► Na+Ca+2 + B509 + 8 H20 Borax is dissolved in water and sodium tetraborate dissociating into ions: NaCa Β 5 0 9 · 8 H 2 0 + Ca +2 ► Na + B 5 0 9 + 8 H 2 0
El ion tetraborato se hidroliza en el agua a ion hidroxilo y acido bórico: The tetraborate ion is hydrolyzed in water to hydroxyl ion and boric acid:
B5O9 + 8 H20 «—► H3BO3 + 20H B5O9 + 8 H 2 0 «—► H3BO3 + 20H
El H2SO4 neutraliza el ion hidroxilo formado, desplazando el equilibrio hacia la derecha: H2SO4 neutralizes the hydroxyl ion formed, shifting the balance to the right:
H2S04 + 2 OH ► 2 H20 + S04 = H 2 S0 4 + 2 OH ► 2 H 2 0 + S0 4 =
Agrupando estas tres ecuaciones, en una sola ecuación general: Grouping these three equations into a single general equation:
2NaCa B509 8H20+ 4H20 + 3H2S04 ► IOH3BO3 + Na2S04 +2 CaS04 2NaCa B 5 0 9 8H 2 0+ 4H 2 0 + 3H 2 S0 4 ► IOH 3 BO 3 + Na 2 S0 4 +2 CaS0 4
Por otra parte, además se puede resumir que en el proceso de obtención de Acido bórico del arte previo a partir del Mineral Bórax, se encuentran implícitas las siguientes reacciones:  On the other hand, it can also be summarized that in the process of obtaining Boric Acid from the prior art from Borax Mineral, the following reactions are implicit:
El Bórax se disuelve en el agua y se disocia a iones sodio y tetraborato: Na2B407—► 2 a++ B407 = Borax is dissolved in water dissociates and sodium tetraborate ions: Na 2 B 4 0 7 -► 2 + B 4 0 7 =
El ion tetraborato se hidroliza en el agua a ion hidroxilo y acido bórico: The tetraborate ion is hydrolyzed in water to hydroxyl ion and boric acid:
B*07 = + H20 ^ H3B03 + 2 OH El H2SO4 neutraliza el ion hidroxilo formado y desplaza el equilibrio hacia la derecha: B * 0 7 = + H 2 0 ^ H 3 B0 3 + 2 OH H2SO4 neutralizes the formed hydroxyl ion and shifts the equilibrium to the right:
H2SO4 + 2 OH" ► 2 II20 + S04 = H2SO4 + 2 OH " ► 2 II 2 0 + S0 4 =
Agrupando estas tres ecuaciones, en una sola ecuación general:  Grouping these three equations into a single general equation:
Na2R+07 + S H20 + H2S04 ». 4 H3RO3 + Na2S04 Na 2 R + 07 + SH 2 0 + H 2 S0 4 '. 4 H3RO3 + Na 2 S0 4
El objeto de la invención es mejorar todos los apartados anteriormente expuestos, modificando el actual proceso productivo en la obtención de Acido Bórico, a partir de salmueras naturales o industriales, o de minerales como la Ulexita y el Bórax, ya que la presente invención actúa directamente sobre el boro contenido en las fuentes antes indicadas precipitando de forma inmediata el bórax en acido bórico. The object of the invention is to improve all the above-mentioned sections, modifying the current production process in obtaining Boric Acid, from natural or industrial brines, or from minerals such as Ulexite and Borax, since the present invention acts directly on the boron contained in the aforementioned sources immediately precipitating the borax in boric acid.
DESCRIPCION DE LAS FIGURAS DESCRIPTION OF THE FIGURES
Figura 1, representa un esquema del proceso de la invención, para la obtención de ácido bórico, a partir de salmuera. Figure 1 represents a scheme of the process of the invention, for obtaining boric acid, from brine.
Figura 2, representa un esquema del proceso de la invención, para la obtención de ácido bórico, a partir de Ulexita. Figura 3, representa un esquema del proceso de la invención, para la obtención de ácido bórico, a partir de Bórax. Figure 2 represents a scheme of the process of the invention, for obtaining boric acid, from Ulexite. Figure 3 represents a scheme of the process of the invention, for obtaining boric acid, from Borax.
DESCRIPCION DETALLADA DE LA INVENCION DETAILED DESCRIPTION OF THE INVENTION
De acuerdo con la invención, los problemas anteriormente reseñados se resuelven mediante la utilización del extractante inorgánico, que es el objetivo principal de la presente invención. El extractante inorgánico de la presente invención está compuesto por las sales de Bario solubles, arriba indicadas, de preferencia Cloruro de Bario (BaCl2). Esta sal de Bario es la que permite precipitar el boro, en base a las propiedades químicas del Boro, que exhibe como característica ventajosa para el propósito de esta invención, el cual es capaz de reaccionar de manera similar a un metal, a pesar de no ser un metal. According to the invention, the problems described above are solved by the use of the inorganic extractant, which is the main objective of the present invention. The inorganic extractant of the present invention is composed of the soluble barium salts, indicated above, preferably Barium Chloride (BaCl 2 ). This salt of Barium is what allows boron to precipitate, based on the chemical properties of Boron, which exhibits as an advantageous characteristic for the purpose of this invention, which is capable of reacting in a similar way to a metal, despite not Be a metal.
La sal utilizada en la presente invención, una sal de bario soluble en agua, de preferencia cloruro de bario, exhibe características que permiten su aplicación en el proceso de la presente invención, siendo una de ellas su solubilidad en agua que es de 35%, y un peso molecular de 208,24, entre otras. En una modalidad de la presente invención, el extractante inorgánico se aplica en el proceso de la presente invención mediante la siguiente secuencia de etapas consecutivas: The salt used in the present invention, a water soluble barium salt, preferably barium chloride, exhibits characteristics that allow its application in the process of the present invention, one of which is its solubility in water which is 35%, and a molecular weight of 208.24, among others. In one embodiment of the present invention, the inorganic extractant is applied in the process of the present invention by the following sequence of consecutive steps:
Se vierte el extractante inorgánico BaCl2, directamente sobre la salmuera de origen natural, mineral o industrial, o bien sobre una solución/suspensión de mineral que contiene B, sin necesidad de ajustar la acidez de la fuente de boro, iniciándose una precipitación selectiva de Borato de Bario, la cual se completa mediante agitación mecánica, según la siguiente reacción, en el caso de realizar la extracción a partir de: a) una salmuera natural o industrial: The inorganic extractant BaCl 2 is poured, directly on the brine of natural, mineral or industrial origin, or on a solution / suspension of mineral containing B, without the need to adjust the acidity of the boron source, initiating a selective precipitation of Barium borate, which is completed by mechanical agitation, according to the following reaction, in the case of extraction from: a) a natural or industrial brine:
BaCl2 + 2H3B03 ► 2 + 2H20 + 2HC1BaCl 2 + 2H 3 B0 3 ► 2 + 2H 2 0 + 2HC1
Figure imgf000013_0001
Figure imgf000013_0001
El precipitado de Borato de Bario obtenido, se disuelve mediante adición de agua caliente, a una temperatura comprendida entre 80 a 98°C, preferentemente entre 82 a 95°C, más preferentemente a 92°C, hasta obtener una solución que comprende una concentración de alrededor de 25% a 40% p/v, preferentemente de 28 a 35%, más preferentemente de 30% de Borato de Bario, la cual se agita mecánicamente, hidrolizándose dicho Borato de Bario para formar Acido bórico, y permitir retirar el bario en forma de un precipitado de sulfato de bario, mediante la adición de ácido sulfúrico en una proporción comprendida entre 1 :2 a 1 :3 de precipitado en solución:ácido sulfúrico concentrado (H2S04c), donde el Acido bórico se obtiene con una pureza de 99,5%, según la siguiente reacción: Ba (BO)2 + 2H20 + H2S0 + 2H3B03 .The precipitate of Barium Borate obtained is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration is obtained from about 25% to 40% w / v, preferably from 28 to 35%, more preferably from 30% Barium Borate, which is mechanically stirred, said Barium Borate being hydrolyzed to form Boric acid, and allow the removal of barium in the form of a precipitate of barium sulfate, by adding sulfuric acid in a proportion between 1: 2 to 1: 3 of precipitate in solution: concentrated sulfuric acid (H 2 S0 4 c), where Boric acid is obtained with a purity of 99.5%, according to the following reaction: Ba (BO) 2 + 2H 2 0 + H 2 S0 + 2H 3 B0 3 .
Figure imgf000014_0001
un mineral de Bórax:
Figure imgf000014_0001
a Borax mineral:
El mineral primero se debe proveer en estado particulado, para lo cual se muele preferentemente hasta alcanzar un tamaño igual o inferior a 15 mm. Enseguida este material particulado se suspende en agua a 30°C hasta obtener una solución al 20% p/v de mineral, agitándose de manera mecánica durante un período de 15 a 30 min, hasta alcanzar la disolución total, posteriormente se adiciona el extractante inorgánico de BaCl2, en proporción estequiométrica, siempre en agitación, provocándose la siguiente reacción: The mineral must first be supplied in a particulate state, for which it is preferably ground to a size equal to or less than 15 mm. Then, this particulate material is suspended in water at 30 ° C until a 20% w / v solution of mineral is obtained, stirring mechanically for a period of 15 to 30 min, until reaching the total solution, then the inorganic extractant is added of BaCl 2 , in stoichiometric proportion, always under stirring, causing the following reaction:
(Na2B4O7«10H2O) + BaCl2 ► BaB4Q7 + 2NaCl + 10 HzO (Na 2 B 4 O 7 '10H 2 O) + BaCl 2 ► BaB 4 2NaCl + Q 7 + 10 H z O
Permitiéndose que repose la mezcla de reacción en precipitación durante 15 a 30 min, para proceder a su posterior filtración, siendo retenido en el filtrado el precipitado de Tetraborato de Bario. El precipitado de la sal de Boro obtenido, se disuelve agregando agua caliente, a una temperatura comprendida entre 80 a 98°C, preferentemente entre 82 a 95°C, más preferentemente a 92 °C, hasta obtener una solución que comprende una concentración de alrededor de 25% a 40% p/v, preferentemente de 28 a 35%, más preferentemente de 30% de Tetraborato de Bario, se mantiene esta solución en agitación hidrolizándose dicho Tetraborato de Bario para formar Acido bórico, y permitir retirar el bario en forma de un precipitado de sulfato de bario, mediante la adición de ácido sulfúrico en una proporción comprendida entre 1 :2 a 1 :3 de precipitado en solución:ácido sulfúrico concentrado (H2SO4C), donde el Acido bórico se obtiene con una pureza de 99,5%, según la siguiente reacción: BaB407 + 5H20 + H2SO4 ► + 4 H3B03 Allowing the reaction mixture to stand in precipitation for 15 to 30 min, to proceed with its subsequent filtration, the precipitate of Barium Tetraborate being retained in the filtrate. The precipitate of the Boron salt obtained is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration of about 25% to 40% w / v, preferably 28 to 35%, more preferably 30% Barium Tetraborate, this solution is kept under stirring, said Tetraborate being hydrolyzed. Barium to form Boric acid, and to allow the removal of barium as a precipitate of barium sulfate, by adding sulfuric acid in a proportion between 1: 2 to 1: 3 of precipitate in solution: concentrated sulfuric acid (H2SO4C) , where Boric acid is obtained with a purity of 99.5%, according to the following reaction: BaB 4 0 7 + 5H 2 0 + H2SO4 ► + 4 H 3 B0 3
Figure imgf000015_0001
c) un mineral de Ulexita:
Figure imgf000015_0001
c) a Ulexite mineral:
El mineral primero se debe proveer en estado particulado, para lo cual se muele preferentemente hasta alcanzar un tamaño igual o inferior a 15 mm. Enseguida este material particulado se suspende en agua a 30°C hasta obtener una solución al 20% p/v de mineral, agitándose de manera mecánica durante un período de 15 a 30 min, hasta alcanzar la disolución total, posteriormente se adiciona el extractante inorgánico de BaCl2, en proporción estequiométrica, siempre en agitación, provocándose la siguiente reacción: The mineral must first be supplied in a particulate state, for which it is preferably ground to a size equal to or less than 15 mm. Then, this particulate material is suspended in water at 30 ° C until a 20% w / v solution of mineral is obtained, stirring mechanically for a period of 15 to 30 min, until reaching the total solution, then the inorganic extractant is added of BaCl 2 , in stoichiometric proportion, always under stirring, causing the following reaction:
2NaCaB509 «8H20 + 3BaCl2 ► + 2NaCl + 2CaCl2 + 8H202NaCaB 5 0 9 « 8H 2 0 + 3BaCl 2 ► + 2NaCl + 2CaCl 2 + 8H 2 0
Figure imgf000015_0002
Figure imgf000015_0002
Permitiéndose que repose la mezcla de reacción en precipitación durante 15 a 30 min, para proceder a su posterior filtración, siendo retenido en el filtrado el precipitado de Pentaborato deAllowing the reaction mixture to stand in precipitation for 15 to 30 min, to proceed with its subsequent filtration, the Pentaborate precipitate being retained in the filtrate.
Bario. El precipitado de la sal de Boro obtenido, se disuelve agregando agua caliente, a una temperatura comprendida entre 80 a 98°C, preferentemente entre 82 a 95°C, más preferentemente a 92°C, hasta obtener una solución que comprende una concentración de alrededor de 25% a 40% p/v, preferentemente de 28 a 35%, más preferentemente de 30% deBarium. The precipitate of the Boron salt obtained is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration of about 25% to 40% w / v, preferably 28 to 35%, more preferably 30% of
Pentaborato de Bario, se mantiene esta solución en agitación hidrolizándose dicho Pentaborato de Bario para formar Acido bórico, y permitir retirar el bario en forma de un precipitado de sulfato de bario, mediante la adición de ácido sulfúrico en una proporción comprendida entre 1 :2 a 1 :3 de precipitado en solución:ácido sulfúrico concentrado (H2S0 c), donde el Acido bórico se obtiene con una pureza de 99,5%, según la siguiente reacción: Barium Pentaborate, this solution is kept under stirring, said Barium Pentaborate being hydrolyzed to form Boric acid, and allowing the removal of barium as a precipitate of barium sulfate, by the addition of sulfuric acid in a ratio between 1: 2 at 1: 3 of precipitate in solution: concentrated sulfuric acid (H 2 S0 c), where Boric acid is obtained with a purity of 99.5%, according to the following reaction:
Ba3(B509)2 + 12H20 + 3 H2S04 + IOH3BO3
Figure imgf000016_0001
Ba 3 (B 5 0 9 ) 2 + 12H 2 0 + 3 H 2 S0 4 + IOH3BO3
Figure imgf000016_0001
El extractante inorgánico BaCl2 utilizado en la presente invención se puede adicionar en forma de una solución acuosa previamente preparada o bien ser preparado in situ al momento de la adición sobre la salmuera o solución de mineral de la cual se desea extraer el boro presente. Este extractante permite una precipitación selectiva del componente Boro contenido en la solución que se someta al proceso de extracción, por lo cual incluso a muy bajas concentraciones exhibe el efecto de inducir la precipitación de boratos, sin embargo, para un efecto práctico de reproducibilidad se prefiere que la razón del extractante en la mezcla de reacción final, esté comprendida entre un 1 a 10% p/v, preferentemente entre un 2 a un 7%, más preferentemente entre un 2,5 a un 4,5%, mucho más preferentemente en una razón de 3% p/v. The inorganic BaCl 2 extractant used in the present invention can be added in the form of a previously prepared aqueous solution or be prepared in situ at the time of addition on the brine or mineral solution from which it is desired to extract the boron present. This extractant allows a selective precipitation of the Boron component contained in the solution that is subjected to the extraction process, so even at very low concentrations it exhibits the effect of inducing the precipitation of borates, however, for a practical reproducibility effect it is preferred that the ratio of the extractant in the final reaction mixture is between 1 to 10% w / v, preferably between 2 to 7%, more preferably between 2.5 to 4.5%, much more preferably at a rate of 3% w / v.
Por lo anterior, es posible considerar que el proceso de la presente invención exhibe los siguientes aspectos ventajosos, por ejemplo para su aplicación en la producción de Li a partir de salmueras naturales, con contenido de boro, donde la separación del boro resulta más efectiva, tanto en tiempo como en la separación selectiva y no contaminante de la misma, además de exhibir grandes ventajas económicas para el proceso global. Therefore, it is possible to consider that the process of the present invention exhibits the following advantageous aspects, for example for its application in the production of Li from natural brines, with boron content, where boron separation is most effective, both in time and in the selective and non-polluting separation of it, in addition to exhibiting great economic advantages for the global process.
El proceso de la presente invención involucra el uso del mencionado extractante de Cloruro de Bario, que permite extraer directamente el Boro de las salmueras naturales o industriales y/o de minerales, independiente de variables como son  The process of the present invention involves the use of said Barium Chloride extractant, which allows the Boron to be extracted directly from natural or industrial brines and / or from minerals, independent of variables such as
- el pH, - la presencia de iones en la salmuera o solución, - the pH, - the presence of ions in the brine or solution,
- la temperatura del proceso.  - process temperature.
Lo cual permite establecer las siguientes diferencias en aspectos que hasta la actualidad representan un problema en la industria del litio:  Which allows to establish the following differences in aspects that until now represent a problem in the lithium industry:
1.- Al ser un proceso que no requiere de extractantes orgánicos para la separación de boro de la salmuera natural: 1.- Being a process that does not require organic extractants for the separation of boron from natural brine:
- Se genera un ahorro económico relevante, por la reducción drástica de la necesidad de agua, en el proceso industrial  - A relevant economic saving is generated, due to the drastic reduction in the need for water, in the industrial process
- se evitan riesgos implícitos en el manejo de solventes como son las delicadas condiciones de almacenaje, manipulación, la inflamación del solvente y los efectos tóxicos, tanto para el ambiente, como para las personas,  - implicit risks are avoided in the handling of solvents such as the delicate conditions of storage, handling, inflammation of the solvent and toxic effects, both for the environment and for people,
- se evita la instalación de un sistema de acumulo de soluciones involucradas en la extracción, en pozas para llevar a cabo la evaporación solar, eliminando el riesgo de filtración,  - the installation of a system of accumulation of solutions involved in the extraction, in wells to carry out the solar evaporation, eliminating the risk of filtration is avoided,
- no se requiere de protocolos adecuados para la eliminación de riles, independizando el proceso de los efectos de contaminación ambiental,  - adequate protocols for the elimination of riles are not required, making the process independent of the effects of environmental pollution,
- la rápida extracción del Boro, acelera el tiempo total del proceso, permitiendo un aumento de la producción diaria. DESCRIPCION DE LA INVENCION  - The rapid extraction of Boron accelerates the total process time, allowing an increase in daily production. DESCRIPTION OF THE INVENTION
La presente invención se relaciona con la obtención de ácido bórico proveniente de salmueras naturales o industriales y/o de minerales, mediante un nuevo proceso de precipitación de compuestos de boro. The present invention relates to the production of boric acid from natural or industrial brines and / or minerals, by means of a new precipitation process of boron compounds.
El proceso de la presente invención se puede aplicar sobre una salmuera natural o industrial, independiente de su origen geográfico que presente una composición que exhiba contenido de boro. También es aplicable dicho proceso sobre soluciones/suspensiones acuosas de minerales, tales como Ulexita y Bórax. The process of the present invention can be applied on a natural or industrial brine, independent of its geographical origin that has a composition that exhibits content of boron. This process is also applicable to aqueous solutions / suspensions of minerals, such as Ulexite and Borax.
Para llevar a cabo dicho proceso, no se requiere de un ajuste de acidez de la salmuera o solución/suspensión, ni de un acondicionamiento térmico de la misma.  In order to carry out said process, an adjustment of acidity of the brine or solution / suspension, nor a thermal conditioning thereof, is not required.
El volumen original de la salmuera tratada o de la o solución/suspensión, de la cual opcionalmente se pueden haber extraído las sales de descarte, se introduce en un Reactor (alrededor de 1500 a 3000 L) en general a temperatura ambiente, en un rango comprendido entre 5°C y +50°C. The original volume of the treated brine or of the solution or suspension, from which the discard salts may optionally have been extracted, is introduced into a Reactor (about 1500 to 3000 L) in general at room temperature, in a range between 5 ° C and + 50 ° C.
Sobre este material de salmuera depositado en un primer reactor, se adiciona el extractante inorgánico, a una concentración final de alrededor de 3% p/v.  On this brine material deposited in a first reactor, the inorganic extractant is added, at a final concentration of about 3% w / v.
Esta mezcla contenida en dicho primer reactor se agita por un período determinado de hasta 1 hora, preferentemente entre 15 y 45 minutos, más preferentemente entre 15 y 30 minutos, para luego permitir un tiempo de reposo de alrededor de 30 minutos, luego del cual se obtendrá en primer lugar la precipitación de Boro, el cual será posteriormente sometido a una purificación y extracción final de ácido bórico, lo que permite obtener este producto con una pureza del 99,5% y un contenido de agua inferior a 0,5%.  This mixture contained in said first reactor is stirred for a certain period of up to 1 hour, preferably between 15 and 45 minutes, more preferably between 15 and 30 minutes, and then allow a stand-by time of about 30 minutes, after which First, Boron precipitation will be obtained, which will be subsequently subjected to a purification and final extraction of boric acid, which allows obtaining this product with a purity of 99.5% and a water content of less than 0.5%.
Una salmuera adecuada para someter al procedimiento de extracción de la presente invención, es aquella de origen natural o industrial que cumple con exhibir cualquier contenido de boro, especialmente un contenido comprendido entre 3000 a 10000 ppm de B, preferentemente de 7000 a 9000 ppm, más preferentemente aquella que contiene 8000 ppm de Boro.  A brine suitable for subjecting to the extraction process of the present invention is that of natural or industrial origin that complies with exhibiting any boron content, especially a content between 3000 to 10,000 ppm of B, preferably 7,000 to 9,000 ppm, more preferably one that contains 8000 ppm of Boron.
En una modalidad preferida de la invención, el procedimiento de extracción de Boro, se puede llevar a cabo en una salmuera de origen natural o industrial, tal como se describe a continuación, a través de los ejemplos específicos que representan las modalidades preferidas de la invención, no entendiéndose que dichos ejemplos se entreguen orientados a limitar el espectro a su mera aplicación, sino que la invención puede ser llevada a cabo como modalidades diferentes a través de la descripción entregada en el presente documento y el conocimiento de rutina del experto medio en el arte. In a preferred embodiment of the invention, the Boron extraction process can be carried out in a brine of natural or industrial origin, as described below, through the specific examples representing the preferred embodiments of the invention. , it being understood that said examples are delivered oriented to limit the spectrum to its mere application, but that the invention can be carried out as different modalities through of the description given in this document and the routine knowledge of the average expert in the art.
Por otra parte, cabe mencionar en caso de ser necesario una detección cualitativa o cuantitativa de la presencia del extractante, la sal de bario soluble, en el producto final, un experto de nivel medio en el arte, estará preparado mediante sus conocimientos para detectar y cuantificar la presencia de dicho elemento principal del extractante inorgánico, el Bario, contenido en el producto final producido con el método para el cual se busca protección en la presente solicitud. El cual a pesar de estar presente en mínimas cantidades, por la alta pureza con que se obtiene el producto final, ácido bórico, pudiese estar presente como un elemento traza o incluso como un elemento ultra-traza que es posible detectar tanto a través de técnicas rutinarias de química cuantitativa como de análisis espectrométricos de última generación como por ejemplo espectrometría de masas con plasma de acoplamiento inductivo (ICP-MS), espectrometría de absorción atómica en horno de grafito (GFAAS), o espectrometría de absorción atómica con llama (FAAS), en caso de ser necesario establecer la presencia del precipitante o bien estimar cuantitativamente la cantidad contenida en el producto final. On the other hand, it is worth mentioning if a qualitative or quantitative detection of the presence of the extractant is necessary, the soluble barium salt, in the final product, a mid-level expert in the art, will be prepared through its knowledge to detect and quantify the presence of said main element of the inorganic extractant, Barium, contained in the final product produced with the method for which protection is sought in the present application. Which in spite of being present in minimal quantities, due to the high purity with which the final product, boric acid, could be present as a trace element or even as an ultra-trace element that can be detected both through techniques Routine quantitative chemistry such as state-of-the-art spectrometric analysis such as inductive coupling plasma mass spectrometry (ICP-MS), graphite furnace atomic absorption spectrometry (GFAAS), or flame atomic absorption spectrometry (FAAS) , in case it is necessary to establish the presence of the precipitant or to estimate quantitatively the amount contained in the final product.
Los siguientes ejemplos se describen a modo de realizaciones preferidas del método de la presente solicitud, y no deberán ser considerados como una limitación a la invención.  The following examples are described by way of preferred embodiments of the method of the present application, and should not be considered as a limitation on the invention.
Ejemplos Examples
Ejemplo 1 Example 1
Extracción de boro utilizando Cloruro de Bario desde una salmuera, de origen natural  Boron extraction using Barium Chloride from a brine, of natural origin
1. Se carga una salmuera en el Reactor 1, de acuerdo al esquema de la Figura 1, y se añade directamente el extractante inorgánico o BaCl2, a temperatura ambiente, en una proporción estequiométrica, que equivale a un 3% final en el volumen de reacción; 2. Se agita de manera mecánica en el fondo del reactor, durante un período comprendido entre 15 a 30 minutos; 1. A brine is loaded into Reactor 1, according to the scheme of Figure 1, and the inorganic extractant or BaCl 2 is added directly, at room temperature, in a stoichiometric proportion, equivalent to a final 3% in volume of reaction; 2. It is mechanically stirred at the bottom of the reactor, for a period between 15 to 30 minutes;
3. Se deja reposar la mezcla obtenida en la etapa anterior por un período comprendido entre 15 a 30 minutos;  3. The mixture obtained in the previous stage is allowed to stand for a period between 15 to 30 minutes;
4. Se obtiene un precipitado 1 de Boro y una solución liquida (Filtrado 1). Posteriormente, es posible proceder a la obtención de Acido Bórico, a partir del precipitado obtenido en la etapa 4 antes indicada, como se detalla a continuación:  4. A Boron precipitate 1 and a liquid solution are obtained (Filtrate 1). Subsequently, it is possible to proceed to obtain Boric Acid, from the precipitate obtained in stage 4 above, as detailed below:
5. Se filtra el Precipitado 1 obtenido, a través de 5 mesh, para luego conducirlo hacia el reactor 2, con un capacidad en volumen de alrededor de 2.000 litros, a temperatura ambiente,  5. The precipitate 1 obtained is filtered, through 5 mesh, to then lead it to reactor 2, with a volume capacity of about 2,000 liters, at room temperature,
6. Se agrega al reactor 2, agua a una temperatura de comprendida entre alrededor de 80 a 95°C, preferentemente a 92 °C, para obtener una solución que contiene como máximo un 30% de acido bórico.  6. Water is added to reactor 2 at a temperature of between about 80 to 95 ° C, preferably at 92 ° C, to obtain a solution containing a maximum of 30% boric acid.
7. La mezcla anterior se agitará con agitador mecánico, en su parte inferior, por un período comprendido entre 15 a 30 minutos,  7. The previous mixture shall be stirred with a mechanical stirrer, in its lower part, for a period between 15 to 30 minutes,
8. Adicionar H2S04 concentrado en una razón de 1 :2,2 de precipitado disuelto en la etapa 5:ácido sulfúrico, para obtener un Precipitado 2; 8. Add concentrated H 2 S0 4 at a ratio of 1: 2.2 precipitate dissolved in step 5: sulfuric acid, to obtain a Precipitate 2;
9. Filtrar el Precipitado 2, que corresponde a un sólido remanente que comprende BaS04;9. Filter the Precipitate 2, which corresponds to a remaining solid comprising BaS0 4 ;
10. Secar el Filtrado 2, que comprende el acido bórico, en un Secador Continuo, a una temperatura comprendida entre alrededor de 100 a 150°C, para finalmente obtener acido bórico seco, con un grado de humedad inferior a un 0,5% de agua y con una concentración del 99,5%, 10. Dry the Filtrate 2, which comprises the boric acid, in a Continuous Dryer, at a temperature between about 100 to 150 ° C, to finally obtain dry boric acid, with a humidity degree of less than 0.5% of water and with a concentration of 99.5%,
Posteriormente el Acido Bórico puro obtenido de la última etapa, se envasa, almacena y distribuye. En una modalidad adicional de la presente invención, es posible continuar con el procedimiento a través de etapas adicionales, por ejemplo en el caso de una salmuera natural, si se desea finalmente extraer Magnesio y Iodo, lo cual se puede lograr de una manera más fácil, económica y no contaminante al haber ya precipitado el boro a través del procedimiento de la presente invención. Subsequently, the pure Boric Acid obtained from the last stage is packaged, stored and distributed. In a further embodiment of the present invention, it is possible to continue the process through additional steps, for example in the case of a natural brine, if it is finally desired to extract Magnesium and Iodine, which can be achieved in an easier way. , economical and non-polluting since boron has already precipitated through the process of the present invention.
Ejemplo 2 Example 2
Extracción de Acido Bórico utilizando Cloruro de Bario a partir del mineral Ulexita  Boric Acid Extraction using Barium Chloride from Ulexite ore
El proceso de extracción de boratos o de ácido bórico a partir del mineral de Ulexita, se puede llevar a cabo a través de las siguientes etapas:  The process of extraction of borates or boric acid from Ulexite ore can be carried out through the following stages:
1. Proveer mineral Ulexita para ser sometido a molienda, hasta alcanzar un tamaño inferior o igual a 15 mm,  1. Provide Ulexite ore for grinding, to a size less than or equal to 15 mm,
2. Cargar el Reactor 1, de acuerdo a la Figura 2, que posee una capacidad de 3.000 L, con 2. Load Reactor 1, according to Figure 2, which has a capacity of 3,000 L, with
600 Kg de Ulexita molida y agua a una temperatura de 30°C, hasta alcanzar una solución de 20% p/v de Ulexita, 600 Kg of ground Ulexite and water at a temperature of 30 ° C, until reaching a solution of 20% w / v of Ulexite,
3. Agitar hasta alcanzar la disolución del mineral, al menos durante 15 a 30 minutos, 3. Stir until the mineral dissolves, at least for 15 to 30 minutes,
4. Agregar el extractante inorgánico o BaCl2 hasta alcanzar un 3%, con agitación, 4. Add the inorganic extractant or BaCl 2 until reaching 3%, with stirring,
5. Mantener la agitación mecánica en la parte inferior del reactor que contiene la mezcla, por un período comprendido entre 15 a 30 minutos, hasta alcanzar la disolución total, 5. Maintain the mechanical agitation in the lower part of the reactor containing the mixture, for a period between 15 to 30 minutes, until total dissolution is reached,
6. Permitir que repose la reacción contenida en el reactor 1, por un período comprendido entre 15 y 30 minutos, para obtener un precipitado 1, 6. Allow the reaction contained in reactor 1 to stand, for a period of 15 to 30 minutes, to obtain a precipitate 1,
7. Filtrar el precipitado a través de 5 mesh,  7. Filter the precipitate through 5 mesh,
8. Reservar el agua proveniente de la filtración de la etapa anterior para ser re-utilizada en un nuevo ciclo de este proceso, 9. Cargar el precipitado 1 obtenido de la etapa 6, en el Reactor 2, con capacidad de 2.000 litros, y se adiciona agua a 92 °C, se agita mecánicamente, en su parte inferior, durante 15 a 30 minutos, 8. Reserve the water from the filtration of the previous stage to be reused in a new cycle of this process, 9. Load the precipitate 1 obtained from step 6, in Reactor 2, with a capacity of 2,000 liters, and add water at 92 ° C, stir mechanically, in its lower part, for 15 to 30 minutes,
10. Adicionar H2S04 concentrado en una razón de 1 :2,5 de precipitado cargado en la etapa 9:ácido sulfúrico, para obtener un Precipitado 2; 10. Add concentrated H 2 S0 4 at a ratio of 1: 2.5 of the precipitate loaded in step 9: sulfuric acid, to obtain a Precipitate 2;
11. Filtrar el Precipitado 2, que corresponde a un sólido remanente que comprende BaS04;11. Filter the Precipitate 2, which corresponds to a remaining solid comprising BaS0 4 ;
12. Secar el Filtrado 2, que comprende el acido bórico, en un Secador Continuo, a una temperatura comprendida entre alrededor de 100 a 1 0°C, para finalmente obtener acido bórico seco, con un grado de humedad inferior a un 0,5% de agua y con una concentración del 99,5%. 12. Dry the Filtrate 2, which comprises the boric acid, in a Continuous Dryer, at a temperature between about 100 to 1 0 ° C, to finally obtain dry boric acid, with a humidity degree of less than 0.5 % of water and with a concentration of 99.5%.
Posteriormente el Acido Bórico puro obtenido de la última etapa de este ejemplo, se envasa, almacena y distribuye.  Subsequently, the pure Boric Acid obtained from the last stage of this example is packaged, stored and distributed.
Ejemplo 3 Example 3
Extracción de Acido Bórico utilizando Cloruro de Bario a partir del mineral Bórax Boric Acid Extraction using Barium Chloride from Borax ore
0E1 proceso de extracción de boratos o de ácido bórico a partir del mineral de Bórax se puede llevar a cabo a través de las siguientes etapas:  0E1 process of extraction of borates or boric acid from Borax ore can be carried out through the following stages:
1. Proveer mineral Bórax para ser sometido a molienda, hasta alcanzar un tamaño inferior o igual a 15 mm,  1. Provide Borax ore for grinding, to a size less than or equal to 15 mm,
2. Cargar el Reactor 1 de una capacidad de 3.000 L, con 600 Kg de Bórax molido y agua a una temperatura de 30°C, hasta alcanzar una solución de 20% p/v de Bórax,  2. Load the Reactor 1 with a capacity of 3,000 L, with 600 kg of ground Borax and water at a temperature of 30 ° C, until reaching a solution of 20% w / v of Borax,
3. Agitar hasta alcanzar la disolución del mineral, al menos durante 15 a 30 minutos, 3. Stir until the mineral dissolves, at least for 15 to 30 minutes,
4. Agregar el extractante inorgánico o BaCl2 hasta alcanzar un 3%, con agitación, 4. Add the inorganic extractant or BaCl 2 until reaching 3%, with stirring,
5. Mantener la agitación mecánica en la parte inferior del reactor que contiene la mezcla, por un período comprendido entre 15 a 30 minutos, hasta alcanzar la disolución total, 6. Permitir que repose la reacción contenida en el reactor 1, por un período comprendido entre 15 y 30 minutos, para obtener un precipitado 1. 5. Maintain the mechanical agitation in the lower part of the reactor containing the mixture, for a period between 15 to 30 minutes, until total dissolution is reached, 6. Allow the reaction contained in reactor 1 to stand, for a period between 15 and 30 minutes, to obtain a precipitate 1.
7. Filtrar el precipitado 1 , a través de 5 mesh,  7. Filter the precipitate 1, through 5 mesh,
8. Reservar el agua proveniente de la filtración de la etapa anterior para ser re-utilizada en un nuevo ciclo de este proceso,  8. Reserve the water from the filtration of the previous stage to be reused in a new cycle of this process,
9. Cargar el precipitado 1, obtenido de la etapa 6, en el Reactor 2, con capacidad de 2.000 litros, y se adiciona agua a 92 °C, se agita mecánicamente, en su parte inferior, durante 15 a 30 minutos,  9. Load the precipitate 1, obtained from step 6, into Reactor 2, with a capacity of 2,000 liters, and add water at 92 ° C, stir mechanically, in its lower part, for 15 to 30 minutes,
10. Adicionar H2S04 concentrado a la solución contenida en el Reactor 2, en una razón de 1 :2,7 de precipitado cargado en la etapa 9:ácido sulfúrico, para obtener un Precipitado 2;10. Add concentrated H 2 S0 4 to the solution contained in Reactor 2, in a ratio of 1: 2.7 of the precipitate loaded in step 9: sulfuric acid, to obtain a Precipitate 2;
11. Filtrar el Precipitado 2, que corresponde a un sólido remanente que comprende BaS0 ;11. Filter the Precipitate 2, which corresponds to a remaining solid comprising BaS0;
12. Secar el Filtrado 2, que comprende el acido bórico, en un Secador Continuo, a una temperatura comprendida entre alrededor de 100 a 150°C, para finalmente obtener acido bórico seco, con un grado de humedad inferior a un 0,5% de agua y con una concentración del 99,5%. 12. Dry the Filtrate 2, which comprises the boric acid, in a Continuous Dryer, at a temperature between about 100 to 150 ° C, to finally obtain dry boric acid, with a humidity degree of less than 0.5% of water and with a concentration of 99.5%.
Posteriormente el Acido Bórico puro obtenido de la última etapa de este ejemplo, se envasa, almacena y distribuye.  Subsequently, the pure Boric Acid obtained from the last stage of this example is packaged, stored and distributed.
La presente invención permite una transformar la manera actual en la que trabajan las industrias relacionadas con procesos industriales en los que interviene el boro, al extraer directamente el boro de la salmuera o de los minerales en suspensión o solución, sin realizar dilución alguna, ni el uso de extractantes orgánicos, evitando la generación de residuos industriales líquidos y evitando la eliminación de productos finales contaminantes.  The present invention allows a transformation of the current way in which the industries related to industrial processes in which boron intervenes work, by directly extracting the boron from the brine or the minerals in suspension or solution, without making any dilution, nor the use of organic extractants, avoiding the generation of liquid industrial waste and avoiding the elimination of polluting final products.
Ejemplo 4 Extracción de Acido Bórico utilizando Fosfato de Bario a partir de una salmuera natural o industrial. Example 4 Boric Acid Extraction using Barium Phosphate from a natural or industrial brine.
Ba3(P04)2 + 6 H3BO3 ► 3 Ba(B02)2 +2 H3P04 + 6H20 Se carga una salmuera en un Reactor, y se añade directamente el extractante inorgánico o Ba3(PO)4, a temperatura ambiente, en una proporción estequiométrica, que equivale a un 3% final en el volumen de reacción; se mantiene esta reacción en agitación mecánica en el fondo del reactor, durante alrededor de 15 a 30 minutos; posteriormente se permite que la mezcla obtenida repose por otro período de alrededor de 15 a 30 minutos. Del reposo anterior se obtiene un precipitado de sal de Boro y una solución liquida. Posteriormente, se procede a la aislar la sal sólida de Boro contenida en el precipitado mediante filtración a través de un tamiz (por ejemplo 5 mesh), para luego traspasar este precipitado a un segundo reactor, a temperatura ambiente. A este segundo reactor se adiciona agua a una temperatura de 80 a 98 °C preferentemente entre 82 a 95 °C, más preferentemente a 92 °C, para obtener una solución que contiene entre 25 a 40 %, preferentemente de 28 a 35%, preferentemente 30% de acido bórico. Se mantiene la mezcla de reacción anterior en agitación mecánica, en la parte inferior del segundo reactor durante alrededor de 15 a 30 minutos, posteriormente se adiciona H2S04 c en una razón de 1 :3, preferentemente de 1 :2 de precipitado disuelto: ácido sulfúrico conc, para obtener un segundo Precipitado, este último se aisla mediante filtración, lo cual origina un remanente que comprende BaS04. Se seca este segundo filtrado, el cual comprende el acido bórico, en un secador, por ejemplo un continuo, a una temperatura entre alrededor de 100 a 150°C, para finalmente obtener acido bórico seco, con un grado de humedad inferior a un 0,5% de agua y con una concentración del 99,5%. El Acido Bórico puro obtenido de la última etapa, se envasa y almacena para su posterior utilización y distribución. S BaíBCb + 6H20 +3 H2S0 3 BaS04 + 6 H3BO3 Ba 3 (P0 4 ) 2 + 6 H3BO3 ► 3 Ba (B0 2 ) 2 +2 H 3 P0 4 + 6H 2 0 A brine is loaded into a Reactor, and the inorganic extractant or Ba 3 (PO) 4 is added directly , at room temperature, in a stoichiometric proportion, equivalent to a final 3% in the reaction volume; this reaction is maintained under mechanical stirring at the bottom of the reactor, for about 15 to 30 minutes; subsequently, the obtained mixture is allowed to stand for another period of about 15 to 30 minutes. From the previous rest a precipitate of Boron salt and a liquid solution are obtained. Subsequently, the solid Boron salt contained in the precipitate is isolated by filtration through a sieve (for example 5 mesh), and then transferred this precipitate to a second reactor, at room temperature. To this second reactor water is added at a temperature of 80 to 98 ° C preferably between 82 to 95 ° C, more preferably at 92 ° C, to obtain a solution containing between 25 to 40%, preferably 28 to 35%, preferably 30% boric acid. The above reaction mixture is maintained under mechanical stirring, in the lower part of the second reactor for about 15 to 30 minutes, then H 2 S0 4 c is added in a ratio of 1: 3, preferably 1: 2 of dissolved precipitate. : conc sulfuric acid, to obtain a second precipitate, the latter is isolated by filtration, which causes a remnant comprising BaS0 4 . This second filtrate is dried, which comprises the boric acid, in a dryer, for example a continuous, at a temperature between about 100 to 150 ° C, to finally obtain dry boric acid, with a humidity degree of less than 0 , 5% water and with a concentration of 99.5%. Pure Boric Acid obtained from the last stage is packaged and stored for later use and distribution. S BaíBCb + 6H 2 0 +3 H 2 S0 3 BaS0 4 + 6 H3BO3
Ejemplo 5 Example 5
Extracción de Acido Bórico utilizando Fosfato de Bario, a partir de un mineral de Bórax:  Boric Acid Extraction using Barium Phosphate, from a Borax mineral:
El mineral primero se debe proveer en estado particulado, para lo cual se muele preferentemente hasta alcanzar un tamaño igual o inferior a 15 mm. Enseguida este material particulado se suspende en agua a 30 °C hasta obtener una solución al 20% p/v de mineral, agitándose de manera mecánica durante un periodo de 15 a 30 min, hasta alcanzar la disolución total, posteriormente se adiciona el extractante inorgánico de Ba3(P04)2, en proporción estequiométrica, siempre en agitación, provocándose la siguiente reacción: The mineral must first be supplied in a particulate state, for which it is preferably ground to a size equal to or less than 15 mm. Then this particulate material is suspended in water at 30 ° C until a 20% w / v solution of mineral is obtained, stirring mechanically for a period of 15 to 30 min, until reaching the total solution, then the inorganic extractant is added of Ba 3 (P0 4 ) 2 , in stoichiometric proportion, always under agitation, causing the following reaction:
3 Na2B4O7« 10 H2O + Ba3(P04)2 ► 3 BaB407 + 2 Na3P04 + 10 H20 3 Na 2 B 4 O 7 «10 H 2 O + Ba 3 (P0 4 ) 2 ► 3 BaB 4 0 7 + 2 Na 3 P0 4 + 10 H 2 0
Permitiéndose que repose la mezcla de reacción en precipitación durante 15 a 30 min, para proceder a su posterior filtración, siendo retenido en el filtrado el precipitado de Tetraborato de Bario. El precipitado de la sal de Boro obtenido, se disuelve agregando agua caliente, a una temperatura comprendida entre 80 a 98°C, preferentemente entre 82 a 95°C, más preferentemente a 92°C, hasta obtener una solución que comprende una concentración de alrededor de 25% a 40% p/v, preferentemente de 28 a 35%, más preferentemente de 30% de Tetraborato de Bario, se mantiene esta solución en agitación hidrolizándose dicho Tetraborato de Bario para formar Acido bórico, y permitir retirar el bario en forma de un precipitado de sulfato de bario, mediante la adición de ácido sulfúrico en una proporción comprendida entre 1 :2 a 1 :3 de precipitado en solución: ácido sulfúrico concentrado (H2S04)c donde el Acido bórico se obtiene con una pureza de 99,5%, según la siguiente reacción: Bal¾(>7 + 3H>S04 + 5¾Q > + 12¾BOjAllowing the reaction mixture to stand in precipitation for 15 to 30 min, to proceed with its subsequent filtration, the precipitate of Barium Tetraborate being retained in the filtrate. The precipitate of the Boron salt obtained is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration of around 25% to 40% w / v, preferably 28 to 35%, more preferably 30% Barium Tetraborate, this solution is kept under stirring, said Barium Tetraborate being hydrolyzed to form Boric Acid, and allowing the barium to be removed in form of a precipitate of barium sulfate, by adding sulfuric acid in a proportion between 1: 2 to 1: 3 of precipitate in solution: concentrated sulfuric acid (H 2 S0 4 ) c where boric acid is obtained with a 99.5% purity, according to the following reaction: Bal¾ (> 7 + 3H> S0 4 + 5¾Q> + 12¾BOj
Figure imgf000025_0001
Ejemplo 6
Figure imgf000025_0001
Example 6
Extracción de Acido Bórico utilizando Fosfato de Bario a partir de un mineral de Ukxita  Boric Acid Extraction using Barium Phosphate from a Ukxita mineral
El mineral primero se debe proveer en estado particulado, para lo cual se muele preferentemente hasta alcanzar un tamaño igual o inferior a 15 mm. Enseguida este material particulado se suspende en agua a 30°C hasta obtener una solución al 20% p/v de mineral, agitándose de manera mecánica durante un periodo de 15 a 30 min, hasta alcanzar la disolución total, posteriormente se adiciona el extractante inorgánico de Ba3(P04)2, eiiprc ordónestequiomélrica, siempre en agitación, provocándose la siguiente reacción: The mineral must first be supplied in a particulate state, for which it is preferably ground to a size equal to or less than 15 mm. Then this particulate material is suspended in water at 30 ° C until a 20% w / v solution of mineral is obtained, stirring mechanically for a period of 15 to 30 min, until reaching the total solution, then the inorganic extractant is added of Ba3 (P0 4 ) 2 , eiiprc ordónestequiomerica, always under agitation, causing the following reaction:
6NaCaB5(V8H20 + 3Ba3(P04)2 ► + 2Na3P04 +2Ca3(P04)2 + 48¾06NaCaB 5 (V8H 2 0 + 3Ba 3 (P0 4) 2 + 2Na 3 ► P0 4 + 2 Ca 3 (P0 4) 2 + 48¾0
Figure imgf000026_0001
Figure imgf000026_0001
Permitiéndose que repose la mezcla de reacción en precipitación durante 15 a 30 min, para proceder a su posterior filtración, siendo retenido en el filtrado el precipitado de Pentaborato de Bario. El precipitado de la sal de Boro obtenido, se disuelve agregando agua caliente, a una temperatura comprendida entre 80 a 98°C, preferentemente entre 82 a 95°C, más preferentemente a 92°C, hasta obtener una solución que comprende una concentración de alrededor de 25% a 40% p/v, preferentemente de 28 a 35%, más preferentemente de 30% de Pentaborato de Bario, se mantiene esta solución en agitación hidrolizándose dicho Pentaborato de Bario para formar Acido bórico, y permitir retirar el bario en forma de un precipitado de sulfato de bario, mediante la adición de ácido sulfúrico en una proporción comprendida entre 1 :2 a 1 :3 de precipitado en solución: ácido sulfúrico concentrado H2S04 , donde el Acido bórico se obtiene con una pureza de 99,5%, según la siguiente reacción: Allowing the reaction mixture to stand in precipitation for 15 to 30 min, to proceed with its subsequent filtration, the precipitate of Barium Pentaborate being retained in the filtrate. The precipitate of the Boron salt obtained is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration of around 25% to 40% w / v, preferably 28 to 35%, more preferably 30% Barium Pentaborate, this solution is kept under stirring, said Barium Pentaborate being hydrolyzed to form Boric Acid, and allowing barium to be removed in form of a precipitate of barium sulfate, by adding sulfuric acid in a proportion between 1: 2 to 1: 3 of precipitate in solution: concentrated sulfuric acid H 2 S0 4 , where Boric acid is obtained with a purity of 99.5%, according to the following reaction:
3Β%(Β509)2+ 36H20 + 9H2S¾ S04 + 30H3BQ33Β% (Β 5 0 9) 2 + 36H + 9H 2 0 2 S0 4 + 30H S¾ 3 BQ3
Figure imgf000026_0002
Figure imgf000026_0002
El extractante inorgánico BasíPO^ utilizado en la presente invención se puede adicionar en forma de una solución acuosa previamente preparada o bien ser preparado in situ al momento de la adición sobre la salmuera o solución de mineral de la cual se desea extraer el boro presente. Este extractante permite una precipitación selectiva del componente Boro contenido en la solución que se someta al proceso de extracción, por lo cual incluso a muy bajas concentraciones exhibe el efecto de inducir la precipitación de boratos, sin embargo, para un efecto práctico de reproducibilidad se prefiere que la razón del extractante en la mezcla de reacción final, esté comprendida entre un 1 a 10% p/v, preferentemente entre un 2 a un 7%, más preferentemente entre un 2,5 a un 4,5%, mucho más preferentemente en una razón de 3% p v. The inorganic extractant BasíPO ^ used in the present invention can be added in the form of a previously prepared aqueous solution or be prepared in situ at the time of the addition on the brine or mineral solution from which it is desired to extract the boron present. This extractant allows a selective precipitation of the Boron component contained in the solution that is subjected to the extraction process, so even at very low concentrations it exhibits the effect of inducing the precipitation of borates, however, for a practical reproducibility effect it is preferred that the ratio of the extractant in the final reaction mixture is between 1 to 10% w / v, preferably between 2 to 7%, more preferably between 2.5 to 4.5%, much more preferably in a ratio of 3% p v.
Ejemplo 7 Example 7
Extracción de Acido Bórico utilizando Fluoruro de Bario como precipitante a partir de una salmuera natural o industrial:  Boric Acid Extraction using Barium Fluoride as a precipitant from a natural or industrial brine:
BaF2 + 2H3B03 ► Ba(B02)2 +2HF + 2H20 BaF 2 + 2H 3 B0 3 ► Ba (B0 2) 2 + 2HF + 2H 2 0
Se carga una salmuera en un Reactor, y se añade directamente el extractante inorgánico o BaF2, a temperatura ambiente, en una proporción estequiométrica, que equivale a un 3% final en el volumen de reacción; se mantiene esta reacción en agitación mecánica en el fondo del reactor, durante alrededor de 15 a 30 minutos; posteriormente se permite que la mezcla obtenida repose por otro período de alrededor de 15 a 30 minutos. Del reposo anterior se obtiene un precipitado de sal de Boro y una solución liquida. Posteriormente, se procede a la aislar la sal sólida que contiene Boro comprendida en el precipitado mediante filtración a través de un tamiz (por ejemplo 5 mesh), para luego traspasar este precipitado a un segundo reactor, a temperatura ambiente. A este segundo reactor se adiciona agua a una temperatura de 80 a 98 °C preferentemente entre 82 a 95 °C, más preferentemente a 92 °C, para obtener una solución que contiene entre 25 a 40 %, preferentemente de 28 a 35%, preferentemente 30% de la sal Borato de Bario. Se mantiene la mezcla de reacción anterior en agitación mecánica, en la parte inferior del segundo reactor durante alrededor de 15 a 30 minutos, posteriormente se adiciona H2S04 c en una razón de 1 :3, preferentemente de 1 :2 de precipitado disuelto: ácido sulfúrico conc, para hidrolizar el borato de bario y obtener un segundo precipitado que corresponde a sulfato de bario, y a la vez obtener el ácido bórico disuelto, el cual se aisla mediante filtración, originando un remanente que comprende BaS04. Se seca este segundo filtrado, el cual comprende el acido bórico, en un secador, por ejemplo un continuo, a una temperatura entre alrededor de 100 a 150°C, para finalmente obtener acido bórico seco, con un grado de humedad inferior a un 0,5% de agua y con una concentración del 99,5%, según la reacción que se indica a continuación. El Acido Bórico puro obtenido de la última etapa, se envasa y almacena para su posterior utilización y distribución. A brine is loaded into a Reactor, and the inorganic extractant or BaF 2 is added directly, at room temperature, in a stoichiometric proportion, equivalent to a final 3% in the reaction volume; this reaction is maintained under mechanical stirring at the bottom of the reactor, for about 15 to 30 minutes; subsequently, the obtained mixture is allowed to stand for another period of about 15 to 30 minutes. From the previous rest a precipitate of Boron salt and a liquid solution are obtained. Subsequently, the solid salt containing Boron contained in the precipitate is isolated by filtration through a sieve (for example 5 mesh), and then transferred this precipitate to a second reactor, at room temperature. To this second reactor water is added at a temperature of 80 to 98 ° C preferably between 82 to 95 ° C, more preferably at 92 ° C, to obtain a solution containing between 25 to 40%, preferably 28 to 35%, preferably 30% of the barium borate salt. The previous reaction mixture is maintained under mechanical stirring, in the lower part of the second reactor for about 15 to 30 minutes, then H 2 S0 4 c is added in a ratio of 1: 3, preferably 1: 2 of dissolved precipitate: conc sulfuric acid, to hydrolyze barium borate and obtain a second precipitate corresponding to barium sulfate, and at the same time to obtain the dissolved boric acid, which is isolated by filtration, causing a remnant comprising BaS0 4 . This second filtrate is dried, which comprises the boric acid, in a dryer, for example a continuous, at a temperature between about 100 to 150 ° C, to finally obtain dry boric acid, with a humidity degree of less than 0 , 5% water and with a concentration of 99.5%, according to the reaction indicated below. Pure Boric Acid obtained from the last stage is packaged and stored for later use and distribution.
Ba(B02)2 + 2H20 + ¾S04 BaS04 + 2H3BO3 Ba (B0 2) 2 + 2H 2 0 + ¾S0 4 BaS0 4 + 2H3BO3
Ejemplo 8 Example 8
Extracción de Acido Bórico utilizando Fluoruro de Bario a partir de un mineral de Bórax: Boric Acid Extraction using Barium Fluoride from a Borax mineral:
El mineral primero se debe proveer en estado particulado, para lo cual se muele preferentemente hasta alcanzar un tamaño igual o inferior a 15 mm. Enseguida este material particulado se suspende en agua a 30 °C hasta obtener una solución al 20% p/v de mineral, agitándose de manera mecánica durante un periodo de 15 a 30 min, hasta alcanzar la disolución total, posteriormente se adiciona el extractante inorgánico de Ba F2 , en proporción estequiometrica, siempre en agitación, provocándose la siguiente reacción: The mineral must first be supplied in a particulate state, for which it is preferably ground to a size equal to or less than 15 mm. Then this particulate material is suspended in water at 30 ° C until a 20% w / v solution of mineral is obtained, stirring mechanically for a period of 15 to 30 min, until reaching the total solution, then the inorganic extractant is added of Ba F 2 , in stoichiometric proportion, always under agitation, causing the following reaction:
( a2B4O7-10H2O) + BaF2 2NaF + 10H20(at 2 B 4 O 7 -10H 2 O) + BaF 2 2NaF + 10H 2 0
Figure imgf000028_0001
Permitiéndose que repose la mezcla de reacción en precipitación durante 15 a 30 min, para proceder a su posterior filtración, siendo retenido en el filtrado el precipitado de Tetraborato de Bario. El precipitado de la sal de Boro obtenido, se disuelve agregando agua caliente, a una temperatura comprendida entre 80 a 98°C, preferentemente entre 82 a 95°C, más preferentemente a 92°C, hasta obtener una solución que comprende una concentración de alrededor de 25% a 40% p/v, preferentemente de 28 a 35%, más preferentemente de 30% de Tetraborato de Bario, se mantiene esta solución en agitación hidrolizándose dicho Tetraborato de Bario para formar Acido bórico, y permitir retirar el bario en forma de un precipitado de sulfato de bario, mediante la adición de ácido sulfúrico en una proporción comprendida entre 1 :2 a 1 :3 de precipitado en solución: ácido sulfúrico concentrado (H2SO4) , donde el Acido bórico se obtiene conunapureza de 99,5%, según la siguiente reacción:
Figure imgf000028_0001
Allowing the reaction mixture to stand in precipitation for 15 to 30 min, to proceed with its subsequent filtration, the precipitate of Barium Tetraborate being retained in the filtrate. The precipitate of the Boron salt obtained is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration of around 25% to 40% w / v, preferably 28 to 35%, more preferably 30% Barium Tetraborate, this solution is kept under stirring, said Barium Tetraborate being hydrolyzed to form Boric Acid, and allowing the barium to be removed in form of a precipitate of barium sulfate, by the addition of sulfuric acid in a ratio between 1: 2 to 1: 3 of precipitate in solution: concentrated sulfuric acid (H2SO4), where Boric acid is obtained with a sump of 99.5 %, according to the following reaction:
BaRfh + 5H20 +¾S04 + 4H3BO3BaRfh + 5H20 + ¾S0 4 + 4H3BO3
Figure imgf000029_0001
Figure imgf000029_0001
Ejemplo 9 Example 9
Extracción de Acido Bórico utilizando Fluoruro de Bario a partir de un mineral de L exita: Boric Acid Extraction using Barium Fluoride from a mineral of L success:
El mineral primero se debe proveer en estado particulado, para lo cual se muele preferentemente hasta alcanzar un tamaño igual o inferior a 15 mm. Enseguida este material particulado se suspende en agua a 30°C hasta obtener una solución al 20% p/v de mineral, agitándose de manera mecánica durante un periodo de 15 a 30 min, hasta alcanzar la disolución total, posteriormente se adiciona el extractante inorgánico de BaF2, en proporción estequiométrica, siempre en agitación, provocándose la siguiente reacción: The mineral must first be supplied in a particulate state, for which it is preferably ground to a size equal to or less than 15 mm. Then this particulate material is suspended in water at 30 ° C until a 20% w / v solution of mineral is obtained, stirring mechanically for a period of 15 to 30 min, until reaching the total solution, then the inorganic extractant is added of BaF 2 , in stoichiometric proportion, always under agitation, causing the following reaction:
2NaCaB5(V8H20 + 3BaF2 9)2 + 2NaF + 2Ca F2+ 8H202NaCaB 5 (V8H 2 0 + 3BaF 2 9 ) 2 + 2NaF + 2Ca F 2 + 8H 2 0
Figure imgf000029_0002
Permitiéndose que repose la mezcla de reacción en precipitación durante 15 a 30 min, para proceder a su posterior filtración, siendo retenido en el filtrado el precipitado de Pentaborato de Bario. El precipitado de la sal de Boro obtenido, se disuelve agregando agua caliente, a una temperatura comprendida entre 80 a 98°C, preferentemente entre 82 a 95°C, más preferentemente a 92°C, hasta obtener una solución que comprende una concentración de alrededor de 25% a 40% p/v, preferentemente de 28 a 35%, más preferentemente de 30% de Pentaborato de Bario, se mantiene esta solución en agitación hidrolizándose dicho Pentaborato de Bario para formar Acido bórico, y permitir retirar el bario en forma de un precipitado de sulfato de bario, mediante la adición de ácido sulfúrico en una proporción comprendida entre 1 :2 a 1 :3 de precipitado en solución: ácido sulfúrico concentrado H2S04 , donde el Acido bórico se obtiene con una pureza de 99,5%, según la siguiente reacción:
Figure imgf000029_0002
Allowing the reaction mixture to stand in precipitation for 15 to 30 min, to proceed with its subsequent filtration, the precipitate of Barium Pentaborate being retained in the filtrate. The precipitate of the Boron salt obtained is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration of around 25% to 40% w / v, preferably 28 to 35%, more preferably 30% Barium Pentaborate, this solution is kept under stirring, said Barium Pentaborate being hydrolyzed to form Boric Acid, and allowing barium to be removed in form of a precipitate of barium sulfate, by adding sulfuric acid in a proportion between 1: 2 to 1: 3 of precipitate in solution: concentrated sulfuric acid H 2 S0 4 , where Boric acid is obtained with a purity of 99.5%, according to the following reaction:
Ba 2 ( B 5 0 9 ) 2 + 13 H 20 + 2 H 2 S 0 4 2BaS04 + IOH3BO3Ba 2 (B 5 0 9 ) 2 + 13 H 2 0 + 2 H 2 S 0 4 2BaS0 4 + IOH3BO3
Figure imgf000030_0001
El extractante inorgánico BaF2 utilizado en la presente invención se puede adicionar en forma de una solución acuosa previamente preparada o bien ser preparado in situ al momento de la adición sobre la salmuera o solución de mineral de la cual se desea extraer el boro presente. Este extractante permite una precipitación selectiva del componente Boro contenido en la solución que se someta al proceso de extracción, por lo cual incluso a muy bajas concentraciones exhibe el efecto de inducir la precipitación de boratos, sin embargo, para un efecto práctico de reproducibilidad se prefiere que la razón del extractante en la mezcla de reacción final, esté comprendida entre un 1 a 10% p/v, preferentemente entre un 2 a un 7%, más preferentemente entre un 2,5 a un 4,5%, mucho más preferentemente en una razón de 3% p/v. Ejemplo 10
Figure imgf000030_0001
The inorganic extractant BaF 2 used in the present invention can be added in the form of a previously prepared aqueous solution or be prepared in situ at the time of the addition on the brine or mineral solution from which it is desired to extract the boron present. This extractant allows a selective precipitation of the Boron component contained in the solution that is subjected to the extraction process, so even at very low concentrations it exhibits the effect of inducing the precipitation of borates, however, for a practical reproducibility effect it is preferred that the ratio of the extractant in the final reaction mixture is between 1 to 10% w / v, preferably between 2 to 7%, more preferably between 2.5 to 4.5%, much more preferably at a rate of 3% w / v. Example 10
Extracción de Acido Bórico utilizando Oxido de Bario como precipitante a partir de una salmuera natural o industrial:  Boric Acid Extraction using Barium Oxide as a precipitant from a natural or industrial brine:
BaO + 2HJB0J +► Ba(B0:): + 3¾0 BaO + 2HJB0J + ► Ba (B0:): + 3¾0
Se carga una salmuera en un Reactor, y se añade directamente el extractante inorgánico o BaO, a temperatura ambiente, en una proporción estequiométrica, que equivale a un 3% final en el volumen de reacción; se mantiene esta reacción en agitación mecánica en el fondo del reactor, durante alrededor de 15 a 30 minutos; posteriormente se permite que la mezcla obtenida repose por otro período de alrededor de 15 a 30 minutos. Del reposo anterior se obtiene un precipitado de sal de Boro y una solución liquida. Posteriormente, se procede a la aislar la sal sólida que contiene Boro comprendida en el precipitado mediante filtración a través de un tamiz (por ejemplo 5 mesh), para luego traspasar este precipitado a un segundo reactor, a temperatura ambiente. A este segundo reactor se adiciona agua a una temperatura de 80 a 98 °C preferentemente entre 82 a 95 °C, más preferentemente a 92 °C, para obtener una solución que contiene entre 25 a 40 %, preferentemente de 28 a 35%, preferentemente 30% de la sal Borato de Bario. Se mantiene la mezcla de reacción anterior en agitación mecánica, en la parte inferior del segundo reactor durante alrededor de 15 a 30 minutos, posteriormente se adiciona H2S04 c en una razón de 1 :3, preferentemente de 1 :2 de precipitado disuelto: ácido sulfúrico conc, para hidrolizar el borato de bario y obtener un segundo precipitado que corresponde a sulfato de bario, y a la vez obtener el ácido bórico disuelto, el cual se aisla mediante filtración, originando un remanente que comprende BaS04. Se seca este segundo filtrado, el cual comprende el acido bórico, en un secador, por ejemplo un continuo, a una temperatura entre alrededor de 100 a 150°C, para finalmente obtener acido bórico seco, con un grado de humedad inferior a un 0,5% de agua y con una concentración del 99,5%, según la reacción que se indica a continuación. El Acido Bórico puro obtenido de la última etapa, se envasa y almacena para su posterior utilización y distribución. A brine is loaded into a Reactor, and the inorganic extractant or BaO is added directly, at room temperature, in a stoichiometric proportion, equivalent to a final 3% in the reaction volume; this reaction is maintained under mechanical stirring at the bottom of the reactor, for about 15 to 30 minutes; subsequently, the obtained mixture is allowed to stand for another period of about 15 to 30 minutes. From the previous rest a precipitate of Boron salt and a liquid solution are obtained. Subsequently, the solid salt containing Boron contained in the precipitate is isolated by filtration through a sieve (for example 5 mesh), and then transferred this precipitate to a second reactor, at room temperature. To this second reactor water is added at a temperature of 80 to 98 ° C preferably between 82 to 95 ° C, more preferably at 92 ° C, to obtain a solution containing between 25 to 40%, preferably 28 to 35%, preferably 30% of the barium borate salt. The above reaction mixture is maintained under mechanical stirring, in the lower part of the second reactor for about 15 to 30 minutes, then H 2 S0 4 c is added in a ratio of 1: 3, preferably 1: 2 of dissolved precipitate. : conc sulfuric acid, to hydrolyze barium borate and obtain a second precipitate corresponding to barium sulfate, and at the same time obtain dissolved boric acid, which is isolated by filtration, causing a remnant comprising BaS0 4 . This second filtrate is dried, which comprises the boric acid, in a dryer, for example a continuous, at a temperature between about 100 to 150 ° C, to finally obtain dry boric acid, with a humidity degree of less than 0 ,5% of water and with a concentration of 99.5%, according to the reaction indicated below. Pure Boric Acid obtained from the last stage is packaged and stored for later use and distribution.
Ba(BC>2)2 + 2H20 + H2S04 + 2H3BO3Ba (BC> 2 ) 2 + 2H 2 0 + H 2 S0 4 + 2H3BO3
Figure imgf000032_0001
Figure imgf000032_0001
Ejemplo 11 Example 11
Extracción de Acido Bórico utilizando Oxido de Bario como precipitante a partir de un mineral de Bórax:  Boric Acid Extraction using Barium Oxide as a precipitant from a Borax mineral:
El mineral primero se debe proveer en estado particulado, para lo cual se muele preferentemente hasta alcanzar un tamaño igual o inferior a 15 mm. Enseguida este material particulado se suspende en agua a 30 °C hasta obtener una solución al 20% p/v de mineral, agitándose de manera mecánica durante un periodo de 15 a 30 min, hasta alcanzar la disolución total, posteriormente se adiciona el extractante inorgánico de BaO, en proporción estequiometrica, siempre en agitación, provocándose la siguiente reacción:  The mineral must first be supplied in a particulate state, for which it is preferably ground to a size equal to or less than 15 mm. Immediately this particulate material is suspended in water at 30 ° C until a 20% w / v solution of mineral is obtained, stirring mechanically for a period of 15 to 30 min, until reaching the total solution, then the inorganic extractant is added of BaO, in stoichiometric proportion, always under agitation, causing the following reaction:
(Na2B4(V10H2O) + BaO BaB407 + Na20 + 10 H20 (Na 2 B 4 (V10H 2 O) + BaO BaB 4 0 7 + Na 2 0 + 10 H 2 0
Permitiéndose que repose la mezcla de reacción en precipitación durante 15 a 30 min, para proceder a su posterior filtración, siendo retenido en el filtrado el precipitado de Tetraborato de Bario. El precipitado de la sal de Boro obtenido, se disuelve agregando agua caliente, a una temperatura comprendida entre 80 a 98°C, preferentemente entre 82 a 95°C, más preferentemente a 92°C, hasta obtener una solución que comprende una concentración de alrededor de 25% a 40% p/v, preferentemente de 28 a 35%, más preferentemente de 30% de Tetraborato de Bario, se mantiene esta solución en agitación hidrolizándose dicho Tetraborato de Bario para formar Acido bórico, y permitir retirar el bario en forma de un precipitado de sulfato de bario, mediante la adición de ácido sulfúrico en una proporción comprendida entre 1 :2 a 1 :3 de precipitado en solución: ácido sulfúrico concentrado (H2S04c) , donde el Acido bórico se obtiene con una pureza de 99,5%, según la siguiente reacción: Allowing the reaction mixture to stand in precipitation for 15 to 30 min, to proceed with its subsequent filtration, the precipitate of Barium Tetraborate being retained in the filtrate. The precipitate of the Boron salt obtained is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration of about 25% to 40% w / v, preferably 28 to 35%, more preferably 30% of Barium Tetraborate, this solution is kept under stirring, said Barium Tetraborate being hydrolyzed to form Boric acid, and allowing the removal of barium in the form of a precipitate of barium sulfate, by the addition of sulfuric acid in a proportion between 1: 2 a 1: 3 precipitate in solution: concentrated sulfuric acid (H 2 S0 4 c), where Boric acid is obtained with a purity of 99.5%, according to the following reaction:
BaB407 + 5H20 +H2S04 ► BaS04 + 4 H3BO3 BaB 4 0 7 + 5H 2 0 + H 2 S0 4 ► BaS0 4 + 4 H3BO3
Ejemplo 12 Example 12
Extracción de Acido Bórico utilizando Oxido de Bario como precipitante a partir de un mineral deUlexita: Boric Acid Extraction using Barium Oxide as a precipitant from a Ulexite mineral:
El mineral primero se debe proveer en estado particulado, para lo cual se muele preferentemente hasta alcanzar un tamaño igual o inferior a 15 mm. Enseguida este material particulado se suspende en agua a 30°C hasta obtener una solución al 20% p/v de mineral, agitándose de manera mecánica durante un periodo de 15 a 30 min, hasta alcanzar la disolución total, posteriormente se adiciona el extractante inorgánico de BaO, en proporción estequiométrica, siempre en agitación, provocándose la siguiente reacción:  The mineral must first be supplied in a particulate state, for which it is preferably ground to a size equal to or less than 15 mm. Immediately this particulate material is suspended in water at 30 ° C until a 20% w / v solution of mineral is obtained, stirring mechanically for a period of 15 to 30 min, until reaching the total solution, then the inorganic extractant is added of BaO, in stoichiometric proportion, always under agitation, causing the following reaction:
2NaCaB509 · 8H20 + 3BaO ► )2 + Na2CH2 CaO+8H202NaCaB 5 0 9 · 8H 2 0 + 3BaO ►) 2 + Na 2 CH2 CaO + 8H 2 0
Figure imgf000033_0001
Permitiéndose que repose la mezcla de reacción en precipitación durante 15 a 30 min, para proceder a su posterior filtración, siendo retenido en el filtrado el precipitado de Pentaborato de
Figure imgf000033_0001
Allowing the reaction mixture to stand in precipitation for 15 to 30 min, to proceed with its subsequent filtration, the Pentaborate precipitate being retained in the filtrate.
Bario. El precipitado de la sal de Boro obtenido, se disuelve agregando agua caliente, a una temperatura comprendida entre 80 a 98°C, preferentemente entre 82 a 95°C, más preferentemente a 92°C, hasta obtener una solución que comprende una concentración de alrededor de 25% a 40% p/v, preferentemente de 28 a 35%, más preferentemente de 30% de Pentaborato de Bario, se mantiene esta solución en agitación hidrolizándose dicho Pentaborato de Bario para formar Acido bórico, y permitir retirar el bario en forma de un precipitado de sulfato de bario, mediante la adición de ácido sulfúrico en una proporción comprendida entre 1 :2 a 1 :3 de precipitado en solución: ácido sulfúrico concentrado (H2S04 c) , donde el Acido bórico se obtiene con una pureza de 99,5%, según la siguiente reacción: .0.0 Ba3(B509)2 + 12H20 + 3H2S04 ► 3BaS04 + 10H3BO3 Barium. The precipitate of the Boron salt obtained, is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration of about 25% to 40% w / v, preferably 28 to 35%, more preferably 30% Barium Pentaborate, this solution is kept under stirring, said Barium Pentaborate being hydrolyzed to form Boric Acid, and allowing barium to be removed as a precipitate of barium sulfate, by the addition of sulfuric acid in a proportion between 1: 2 to 1: 3 of precipitate in solution: concentrated sulfuric acid (H 2 S0 4 c), where Boric acid is obtained with a purity 99.5%, according to the following reaction: .0.0 Ba 3 (B 5 0 9 ) 2 + 12H 2 0 + 3H 2 S0 4 ► 3BaS0 4 + 10H 3 BO 3
El extractante inorgánico BaO utilizado en la presente invención se puede adicionar en forma de una solución acuosa previamente preparada o bien ser preparado in situ al momento de la adición sobre la salmuera o solución de mineral de la cual se desea extraer el boro presente. Este extractante permite una precipitación selectiva del componente Boro contenido en la solución que se someta al proceso de extracción, por lo cual incluso a muy bajas concentraciones exhibe el efecto de inducir la precipitación de boratos, sin embargo, para un efecto práctico de reproducibilidad se prefiere que la razón del extractante en la mezcla de reacción final, esté comprendida entre un 1 a 10% p/v, preferentemente entre un 2 a un 7%, más preferentemente entre un 2,5 a un 4,5%, mucho más preferentemente en una razón de 3% p/v. The inorganic BaO extractant used in the present invention can be added in the form of a previously prepared aqueous solution or be prepared in situ at the time of the addition on the brine or mineral solution from which it is desired to extract the boron present. This extractant allows a selective precipitation of the Boron component contained in the solution that is subjected to the extraction process, so even at very low concentrations it exhibits the effect of inducing the precipitation of borates, however, for a practical reproducibility effect it is preferred that the ratio of the extractant in the final reaction mixture is between 1 to 10% w / v, preferably between 2 to 7%, more preferably between 2.5 to 4.5%, much more preferably at a rate of 3% w / v.
Ejemplo 13 Example 13
Extracción de Acido Bórico utilizando Nitrato de Bario como precipitante a partir de una salmuera natural o industrial: Ba(N03)2 + 2Η3ΒΦ, Ba(B02)2 +2HN03 + 2H20 Boric Acid Extraction using Barium Nitrate as a precipitant from a natural or industrial brine: Ba (N0 3 ) 2 + 2Η3ΒΦ, Ba (B0 2 ) 2 + 2HN0 3 + 2H 2 0
Se carga una salmuera en un Reactor, y se añade directamente el extractante inorgánico o Ba(N03)2, a temperatura ambiente, en una proporción estequiométrica, que equivale a un 3% final en el volumen de reacción; se mantiene esta reacción en agitación mecánica en el fondo del reactor, durante alrededor de 15 a 30 minutos; posteriormente se permite que la mezcla obtenida repose por otro período de alrededor de 15 a 30 minutos. Del reposo anterior se obtiene un precipitado de sal de Boro y una solución liquida. Posteriormente, se procede a la aislar la sal sólida que contiene Boro comprendida en el precipitado mediante filtración a través de un tamiz (por ejemplo 5 mesh), para luego traspasar este precipitado a un segundo reactor, a temperatura ambiente. A este segundo reactor se adiciona agua a una temperatura de 80 a 98 °C preferentemente entre 82 a 95 °C, más preferentemente a 92 °C, para obtener una solución que contiene entre 25 a 40 %, preferentemente de 28 a 35%, preferentemente 30% de la sal Borato de Bario. Se mantiene la mezcla de reacción anterior en agitación mecánica, en la parte inferior del segundo reactor durante alrededor de 15 a 30 minutos, posteriormente se adiciona H2S04 c en una razón de 1 :3, preferentemente de 1 :2 de precipitado disuelto: ácido sulfúrico conc, para hidrolizar el borato de bario y obtener un segundo precipitado que corresponde a sulfato de bario, y a la vez obtener el ácido bórico disuelto, el cual se aisla mediante filtración, originando un remanente que comprende BaS04. Se seca este segundo filtrado, el cual comprende el acido bórico, en un secador, por ejemplo un continuo, a una temperatura entre alrededor de 100 a 150°C, para finalmente obtener acido bórico seco, con un grado de humedad inferior a un 0,5% de agua y con una concentración del 99,5%, según la reacción que se indica a continuación. El Acido Bórico puro obtenido de la última etapa, se envasa y almacena para su posterior utilización y distribución. BaíBOi + 2H2O + H2SO4 ► BaS0 + 2HjB03 A brine is loaded into a Reactor, and the inorganic extractant or Ba (N0 3 ) 2 is added directly, at room temperature, in a stoichiometric proportion, equivalent to a final 3% in the reaction volume; this reaction is maintained under mechanical stirring at the bottom of the reactor, for about 15 to 30 minutes; subsequently, the obtained mixture is allowed to stand for another period of about 15 to 30 minutes. From the previous rest a precipitate of Boron salt and a liquid solution are obtained. Subsequently, the solid salt containing Boron contained in the precipitate is isolated by filtration through a sieve (for example 5 mesh), and then transferred this precipitate to a second reactor, at room temperature. To this second reactor water is added at a temperature of 80 to 98 ° C preferably between 82 to 95 ° C, more preferably at 92 ° C, to obtain a solution containing between 25 to 40%, preferably 28 to 35%, preferably 30% of the barium borate salt. The above reaction mixture is maintained under mechanical stirring, in the lower part of the second reactor for about 15 to 30 minutes, then H 2 S0 4 c is added in a ratio of 1: 3, preferably 1: 2 of dissolved precipitate. : conc to hydrolyze the barium borate precipitate and obtain a second corresponding to barium sulfate, while boric acid dissolved obtained, which is isolated by filtration, resulting in a BaS0 4 comprising remnant. This second filtrate is dried, which comprises the boric acid, in a dryer, for example a continuous, at a temperature between about 100 to 150 ° C, to finally obtain dry boric acid, with a humidity degree of less than 0 , 5% water and with a concentration of 99.5%, according to the reaction indicated below. Pure Boric Acid obtained from the last stage is packaged and stored for later use and distribution. BaíBOi + 2H2O + H2SO4 ► BaS0 + 2HjB0 3
Ejemplo 14 Example 14
Extracción de Acido Bórico utilizando Nitrato de Bario como precipitante a partir de un mineral de Bórax: Boric Acid Extraction using Barium Nitrate as a precipitant from a Borax mineral:
El mineral primero se debe proveer en estado particulado, para lo cual se muele preferentemente hasta alcanzar un tamaño igual o inferior a 15 mm. Enseguida este material particulado se suspende en agua a 30 °C hasta obtener una solución al 20% p/v de mineral, agitándose de manera mecánica durante un periodo de 15 a 30 min, hasta alcanzar la disolución total, posteriormente se adiciona el extractante inorgánico de Ba(N03)2, en proporción estequiometrica, siempre en agitación, provocándose la siguiente reacción: The mineral must first be supplied in a particulate state, for which it is preferably ground to a size equal to or less than 15 mm. Then this particulate material is suspended in water at 30 ° C until a 20% w / v solution of mineral is obtained, stirring mechanically for a period of 15 to 30 min, until reaching the total solution, then the inorganic extractant is added of Ba (N0 3 ) 2 , in stoichiometric proportion, always under agitation, causing the following reaction:
(Na2B4O7»10H2O) + Ba(N03>2 ► BaB 07 + 2 NaN03 + 10H20 (Na 2 B 4 O 7 »10H 2 O) + Ba (N0 3 > 2 ► BaB 0 7 + 2 NaN0 3 + 10H 2 0
Permitiéndose que repose la mezcla de reacción en precipitación durante 15 a 30 rnin, para proceder a su posterior filtración, siendo retenido en el filtrado el precipitado de Tetraborato de Bario. El precipitado de la sal de Boro obtenido, se disuelve agregando agua caliente, a una temperatura comprendida entre 80 a 98°C, preferentemente entre 82 a 95°C, más preferentemente a 92°C, hasta obtener una solución que comprende una concentración de alrededor de 25% a 40% p/v, preferentemente de 28 a 35%, más preferentemente de 30% de Tetraborato de Bario, se mantiene esta solución en agitación hidrolizándose dicho Tetraborato de Bario para formar Acido bórico, y permitir retirar el bario en forma de un precipitado de sulfato de bario, mediante la adición de ácido sulfúrico en una proporción comprendida entre 1 :2 a 1 :3 de precipitado en solución: ácido sulfúrico concentrado (H2S04) , donde el Acido bórico se obtiene con una pureza de 99,5%, según la siguiente reacción: BaRfh + 51¼0 +Η 04 ► BaS¾ + 4r¼B(¼ Allowing the reaction mixture to stand in precipitation for 15 to 30 rnin, for subsequent filtration, the precipitate of Barium Tetraborate being retained in the filtrate. The precipitate of the Boron salt obtained is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration of around 25% to 40% w / v, preferably 28 to 35%, more preferably 30% Barium Tetraborate, this solution is kept under stirring, said Barium Tetraborate being hydrolyzed to form Boric Acid, and allowing the barium to be removed in form of a precipitate of barium sulfate, by adding sulfuric acid in a proportion between 1: 2 to 1: 3 of precipitate in solution: concentrated sulfuric acid (H 2 S0 4 ), where Boric acid is obtained with a 99.5% purity, according to the following reaction: BaRfh + 51¼0 + Η 0 4 ► BaS¾ + 4r¼B (¼
Ejemplo 15 Example 15
Extracción de Acido Bórico utilizando Nitrato de Bario como precipitante a partir de un mineral de Ulexita;  Boric Acid Extraction using Barium Nitrate as a precipitant from a Ulexite mineral;
El mineral primero se debe proveer en estado particulado, para lo cual se muele preferentemente hasta alcanzar un tamaño igual o inferior a 15 mm. Enseguida este material particulado se suspende en agua a 30°C hasta obtener una solución al 20% p/v de mineral, agitándose de manera mecánica durante un periodo de 15 a 30 min, hasta alcanzar la disolución total, posteriormente se adiciona el extractante inorgánico de Ba(N03)2 , en proporción estequiométrica, siempre en agitación, provocándose la siguiente reacción: The mineral must first be supplied in a particulate state, for which it is preferably ground to a size equal to or less than 15 mm. Then this particulate material is suspended in water at 30 ° C until a 20% w / v solution of mineral is obtained, stirring mechanically for a period of 15 to 30 min, until reaching the total solution, then the inorganic extractant is added of Ba (N0 3 ) 2 , in stoichiometric proportion, always under agitation, causing the following reaction:
2NaCaB509'8H20 + 3Ba(N03) , ► Ba 3(B 50 9)2 + 2 NaN03 + 2Ca(N03)2 + 8H20 2NaCaB 5 0 9 '8H 2 0 + 3Ba (N0 3 ), ► Ba 3 (B 5 0 9 ) 2 + 2 NaN0 3 + 2Ca (N0 3 ) 2 + 8H 2 0
Permitiéndose que repose la mezcla de reacción en precipitación durante 15 a 30 min, para proceder a su posterior filtración, siendo retenido en el filtrado el precipitado de Pentaborato de Bario. El precipitado de la sal de Boro obtenido, se disuelve agregando agua caliente, a una temperatura comprendida entre 80 a 98°C, preferentemente entre 82 a 95°C, más preferentemente a 92°C, hasta obtener una solución que comprende una concentración de alrededor de 25% a 40% p/v, preferentemente de 28 a 35%, más preferentemente de 30% de Pentaborato de Bario, se mantiene esta solución en agitación hidrolizándose dicho Pentaborato de Bario para formar Acido bórico, y permitir retirar el bario en forma de un precipitado de sulfato de bario, mediante la adición de ácido sulfúrico en una proporción comprendida entre 1 :2 a 1 :3 de precipitado en solución: ácido sulfúrico concentrado (H2S04C) , donde el Acido bórico se obtiene con una pureza de 99,5%, según la siguiente reacción: Allowing the reaction mixture to stand in precipitation for 15 to 30 min, to proceed with its subsequent filtration, the precipitate of Barium Pentaborate being retained in the filtrate. The precipitate of the Boron salt obtained is dissolved by adding hot water, at a temperature between 80 to 98 ° C, preferably between 82 to 95 ° C, more preferably at 92 ° C, until a solution comprising a concentration of around 25% to 40% w / v, preferably 28 to 35%, more preferably 30% Barium Pentaborate, this solution is kept under stirring, said Barium Pentaborate being hydrolyzed to form Boric Acid, and allowing barium to be removed in form of a precipitate of Barium sulfate, by adding sulfuric acid in a proportion between 1: 2 and 1: 3 of precipitate in solution: concentrated sulfuric acid (H2S04C), where Boric acid is obtained with a purity of 99.5%, according to The following reaction:
Ba3(B50t,)2+12H20+3H2S04 ► 3BaS0 + 10H3BO3 Ba3 (B 5 0t,) 2 + 12H20 + 3H2S04 ► 3BaS0 + 10H 3 BO 3
El extractante inorgánico Ba (N03)2 utilizado en la presente invención se puede adicionar en forma de una solución acuosa previamente preparada o bien ser preparado in situ al momento de la adición sobre la salmuera o solución de mineral de la cual se desea extraer el boro presente. Este extractante permite una precipitación selectiva del componente Boro contenido en la solución que se someta al proceso de extracción, por lo cual incluso a muy bajas concentraciones exhibe el efecto de inducir la precipitación de boratos, sin embargo, para un efecto práctico de reproducibilidad se prefiere que la razón del extractante en la mezcla de reacción final, esté comprendida entre un 1 a 10% p/v, preferentemente entre un 2 a un 7%, más preferentemente entre un 2,5 a un 4,5%, mucho más preferentemente en una razón de 3% p/v. The inorganic extractant Ba (N0 3 ) 2 used in the present invention can be added in the form of a previously prepared aqueous solution or be prepared in situ at the time of addition on the brine or mineral solution from which it is desired to extract the Boron present. This extractant allows a selective precipitation of the Boron component contained in the solution that is subjected to the extraction process, so even at very low concentrations it exhibits the effect of inducing the precipitation of borates, however, for a practical reproducibility effect it is preferred that the ratio of the extractant in the final reaction mixture is between 1 to 10% w / v, preferably between 2 to 7%, more preferably between 2.5 to 4.5%, much more preferably at a rate of 3% w / v.

Claims

REIVINDICACIONES
1. Proceso de extracción de Boro a partir de salmueras de origen natural o industrial, o bien del boro contenido en un mineral que contiene B, CARACTERIZADO porque dicho proceso se realiza sin necesidad de ajuste de acidez y libre de solventes, a través de las siguientes etapas: a) proveer una forma de solución acuosa el material que contiene boro de una salmuera natural o industrial, o de una solución/suspensión de un mineral particulado que contiene boro, 1. Boron extraction process from brines of natural or industrial origin, or of the boron contained in a mineral that contains B, CHARACTERIZED because said process is carried out without the need for acidity and solvent-free adjustment, through the following steps: a) provide an aqueous solution form the material containing boron of a natural or industrial brine, or of a solution / suspension of a particulate mineral containing boron,
b) adicionar el extractante, compuesto por una sal de Bario soluble en agua;  b) add the extractant, consisting of a water soluble barium salt;
c) separar el precipitado de borato obtenido de la etapa anterior  c) separate the borate precipitate obtained from the previous step
d) opcionalmente disolver e hidrolizar el precipitado para obtener ácido bórico.  d) optionally dissolve and hydrolyze the precipitate to obtain boric acid.
2. El proceso de extracción de Boro de acuerdo a la reivindicación 1, CARACTERIZADO porque el extractante se selecciona del grupo formado por Cloruro de Bario, Oxido de Bario, Hidróxido de Bario, Fluoruro de Bario, Sulfuro de Bario, Sulfato de Bario, Sulfato de Bario Dihidratado, Sulfito de Bario, Nitrato de Bario, Carbonato de Bario, Fosfato de Bario, Bisulfito de Bario, Hipoclorito de Bario, Clorato de Bario, Peróxido de Bario, Oxicloruro de Bario, Metabisulfíto de Bario, Clorito de Bario, Clorato de Bario2. The Boron extraction process according to claim 1, CHARACTERIZED in that the extractant is selected from the group consisting of Barium Chloride, Barium Oxide, Barium Hydroxide, Barium Fluoride, Barium Sulphide, Barium Sulfate, Sulfate Barium Dihydrate, Barium Sulphite, Barium Nitrate, Barium Carbonate, Barium Phosphate, Barium Hypochlorite, Barium Chlorate, Barium Peroxide, Barium Oxychloride, Barium Metabisulphite, Barium Chlorite, Chlorate Barium
3. El proceso de extracción de Boro de acuerdo a la reivindicación 1, CARACTERIZADO porque el extractante es Cloruro de Bario, el que puede encontrarse en forma anhidra y/o hexahidratada. 3. The Boron extraction process according to claim 1, CHARACTERIZED in that the extractant is Barium Chloride, which can be found in anhydrous and / or hexahydrated form.
4. El proceso de extracción de Boro de acuerdo a la reivindicación 3, CARACTERIZADO porque el cloruro de Bario en la etapa b) se adiciona a la mezcla de reacción en una proporción de BaCl2:mezcla de reacción final, comprendida entre 1 a 10% p/v, preferentemente entre 2 a 7%, más preferentemente entre 2,5 a 4,5%, mucho más preferentemente de de 3% p/v. 4. The Boron extraction process according to claim 3, CHARACTERIZED in that the barium chloride in step b) is added to the reaction mixture in a proportion of BaCl 2 : final reaction mixture, comprised between 1 to 10% w / v, preferably between 2 to 7%, more preferably between 2.5 to 4.5%, much more preferably 3% w / v.
5. El proceso de extracción de Boro de acuerdo a la reivindicación 1 o 3, CARACTERIZADO porque dicha salmuera es de origen natural o industrial. 5. The Boron extraction process according to claim 1 or 3, CHARACTERIZED in that said brine is of natural or industrial origin.
6. El proceso de extracción de Boro de acuerdo a la reivindicación 1 o 3, CARACTERIZADO porque el mineral que contiene boro se selecciona de Ulexita y Bórax. 6. The Boron extraction process according to claim 1 or 3, CHARACTERIZED in that the ore containing boron is selected from Ulexite and Borax.
7. El proceso de extracción de Boro de acuerdo a la reivindicación 1 o 3, CARACTERIZADO porque el mineral particulado, proviene de un mineral ha sido previamente sometido a molienda para alcanzar un tamaño de partícula menor o igual a 15 mm. 7. The Boron extraction process according to claim 1 or 3, CHARACTERIZED because the particulate mineral, comes from a mineral has previously been subjected to grinding to reach a particle size less than or equal to 15 mm.
8. El proceso de extracción de Boro de acuerdo a la reivindicaciones 1 a 3, CARACTERIZADO porque la solución suspensión de dicho mineral particulado que contiene boro, contiene un 20% p/v de dicho mineral. 8. The Boron extraction process according to claims 1 to 3, CHARACTERIZED in that the suspension solution of said particulate mineral containing boron contains 20% w / v of said mineral.
PCT/CL2011/000042 2010-12-17 2011-07-28 Process for obtaining boron from natural or industrial and/or mineral brines that comprise boron, using an inorganic extractant for extracting the boron WO2012079185A1 (en)

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CN103896296A (en) * 2014-03-18 2014-07-02 中国科学院过程工程研究所 Method and device for extracting boron from saline brine by using air-floatation polymers

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