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WO2013053165A1 - Procédé de production de carbonate de lithium par application d'un procédé d'ajout de plusieurs eaux mères et utilisation d'une eau mère de type carbonate et d'une eau mère de type sulfate en tant que matières premières - Google Patents

Procédé de production de carbonate de lithium par application d'un procédé d'ajout de plusieurs eaux mères et utilisation d'une eau mère de type carbonate et d'une eau mère de type sulfate en tant que matières premières Download PDF

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Publication number
WO2013053165A1
WO2013053165A1 PCT/CN2011/082081 CN2011082081W WO2013053165A1 WO 2013053165 A1 WO2013053165 A1 WO 2013053165A1 CN 2011082081 W CN2011082081 W CN 2011082081W WO 2013053165 A1 WO2013053165 A1 WO 2013053165A1
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brine
carbonate
lithium
ions
halogenation
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Chinese (zh)
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陈兆华
陈默
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00—Lithium compounds
    • C01D15/08—Carbonates; Bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00—Compounds of magnesium
    • C01F5/24—Magnesium carbonates

Definitions

  • the invention belongs to the field of inorganic salt chemical industry, and particularly relates to a production method for preparing lithium carbonate by using a double-type halogen method using a carbonate type brine and a sulfate type brine as raw materials.
  • Lithium carbonate has a very high value and a broad market prospect. At present, there are many methods for preparing lithium salt from brine in China and abroad. The main ones are:
  • Brine-thermal decomposition method combine with lime milk to remove sulfate, and then decompose with high temperature furnace to convert magnesium chloride into HC1 and MgO, water-impregnated magnesium oxide residue, and then add soda in the leachate to remove the remaining magnesium ions. Take lithium salt products.
  • the solar pool method uses carbonate-type brine to naturally evaporate to the lithium carbonate in the brine at room temperature, and then moves to the solar pool.
  • the solar water is used to heat the brine. Since the lithium carbonate is in reverse solubility, the solubility decreases as the temperature rises.
  • the principle is to precipitate lithium carbonate in brine.
  • the enrichment of lithium in brine is difficult because the solubility of lithium carbonate is small and reverse solubility, according to the enrichment of lithium in brine in Cambodia salt lake.
  • the saturation content of lithium in the brine in summer is about 1.5 g/l
  • the saturation content of lithium in the brine in winter is about 2. 5 g/l, that is, the natural evaporation amount is large in summer, which is favorable for production, and the solubility of lithium carbonate is small.
  • the solubility of lithium carbonate is not conducive to production, and the solar pool commonly used in industry brings great difficulties to production.
  • lithium in the process of extracting lithium carbonate, lithium can be enriched in brine.
  • lithium ions can be enriched to more than 8g/l, and the highest lithium ion can be obtained. 12g/l, but the separation of magnesium and lithium is a difficult problem in the production of lithium salt in salt chemical industry for many years. Summary of the invention
  • the object of the present invention is to provide a method for producing lithium carbonate by using a double-type halogenated brine and a sulphate-type brine as a raw material for the extraction of lithium carbonate by using the above-mentioned two types of brines in the process of extracting lithium.
  • the object of the invention can be achieved by the following measures:
  • a production method for preparing lithium carbonate by using a double-type halogen method using a carbonate type brine and a sulfate type brine as a raw material comprising the following steps:
  • the lithium-rich brine is concentrated with evaporation to a carbonate-type halogen with a saturated or near-saturated lithium ion concentration.
  • Mixing water, a second Brine, two kinds of adjustment amounts of brine in the brine mixing lithium carbonate Li + ions, solid-liquid separation after completion of the Brine precipitation of lithium carbonate, lithium carbonate obtained precipitate was washed with hot water and Dry to obtain a lithium carbonate product.
  • the method of the present invention may further comprise the following step of halogenating for the third time: the second halogen-completed and solid-liquid separated liquid is combined with the washing liquid after washing the lithium carbonate precipitate, and then mixed with the sulfate-type brine.
  • the amount of the two brines is adjusted to completely react the CO/- ions in the mixed halide with the Mg 2+ ions to form basic magnesium carbonate;
  • the brine after the third halogenation is directly mixed with the brine after the first halogenation, and then concentrated by evaporation, and then solid-liquid separation removes the precipitate of basic magnesium carbonate to obtain lithium enriched brine for the second time.
  • the brine after the third halogenation is first evaporated and concentrated, and the obtained brine is mixed with the brine which is firstly halogenated and evaporated and concentrated, and then subjected to solid-liquid separation to remove the precipitate of basic magnesium carbonate to obtain lithium-rich brine.
  • the brine after the third halogenation is first evaporated and concentrated, and the obtained brine is mixed with the brine which is firstly halogenated and evaporated and concentrated, and then subjected to solid-liquid separation to remove the precipitate of basic magnesium carbonate to obtain lithium-rich brine.
  • the brine after the third halogenation is first evaporated and concentrated, and then the solid magnesium hydroxide precipitate is removed by solid-liquid separation, and the obtained liquid is combined with the lithium-rich brine obtained by the first halogenation to carry out the second halogenation.
  • the method of the present invention can obtain the lithium carbonate product of higher purity and yield only by the steps 1) and 2), but in order to maximize the extraction of lithium in the brine and reduce the discharge of waste water, it can be in step 1) And 2) then add a third process of halogenation.
  • Brine carbonate invention containing C0 3 2 - ions and Li + ions from salt lake brine; brine containing the sulfate type S0 4 2 - ions, Mg 2+ ions and Li + ions from salt lake brine. It is also possible to contain potassium, sodium, and chlorine ions in the two brines.
  • the specific brine composition varies depending on the salt lake.
  • the sulfate type brine in the present invention can also be extended to other types of magnesium containing brine.
  • the two kinds of brines of the invention can be directly used for halogenation, or a brine can be pre-evaporated and concentrated before the first halogenation. Since the brine of most salt lakes of the salt lake brine is unsaturated, it is pre-evaporated and concentrated. It is possible to reduce the amount of brine transported during halogenation. It is of course also possible to pre-evaporate both brines to reduce the water content and to reduce the pressure of subsequent evaporation and concentration.
  • the water may be pre-evaporated to a concentration of co 3 2 - ions at or below a saturated concentration prior to use; the sulfate-type brine may be pre-evaporated to a concentration of Mg 2+ ions at or below a saturated concentration prior to use.
  • step 1 after the completion of the halogenation, the brine is evaporated and concentrated. Since the brine is deficient in the precipitated lithium, the lithium ion can be enriched to a large extent.
  • the content of lithium ions in the water can be greater than 4 g/l, and the concentration of lithium ions is preferably 7.5 to 8.5 g/l. If the concentration is too high, the precipitation of lithium ions is likely to be caused, and if the concentration is too low, the water content in the brine is too large. Increase subsequent production pressure. Therefore, the content of Li+ ions in the lithium-rich brine obtained in the step 1 is preferably 7.5 to 8.5 g/l.
  • the first halogenation process can be carried out at 0 to 90 ° C. In order to save costs and other factors (such as solubility), it is usually at room temperature (20 to 30 ° C).
  • the content of lithium ions in the carbonate-type brine which is concentrated or nearly saturated with lithium ion concentration in the step 2 is generally 1.5 to 2.5 g/l, which is slightly different depending on the specific ambient temperature.
  • the second halogenation can make the lithium-rich brine and the lithium ion in the saturated or near-saturated brine as extracted as possible in the form of lithium carbonate in the case of interference with magnesium ions, that is, to make the lithium in the mixed brine as much as possible.
  • the ions are completely precipitated.
  • the amount of the two brines is adjusted so that the molar amount of C0 3 2 - ions in the mixed brine reacted with Li + ions to form lithium carbonate is 0 to 30%. That is, the amount of carbonate ions added is 100 to 130% of the theoretical amount, and the ratio of halogen is determined. If the amount of carbonate ions is small, the precipitation of lithium carbonate is insufficient, which affects the single-line recovery of lithium. If the amount of carbonate is increased, the precipitation rate of lithium is not lowered, but the amount of carbonate ions is too large, which causes the equipment to operate in an empty manner and affects the equipment capacity.
  • the lithium carbonate obtained by washing with hot water is precipitated, because the solubility of lithium carbonate in water decreases with the increase of temperature, so the hot water can reduce the damage caused by washing and sedimentation.
  • the temperature of the hot water can be adjusted from 30 ° C to 100 ° C. In order to make full use of the local solar energy, it can be washed with solar hot water, and the temperature is generally 75 to 85 ° C.
  • the second halogen can be carried out at 0 to 90 ° C, usually at room temperature (20 to 30 ° C).
  • One solution is to carry out at normal temperature (20 ⁇ 30 ° C) to 85 ° C, especially at 80 ° C or close to 80 V (such as 75 ° C: ⁇ 85 ° C), because The solubility of lithium carbonate at the temperature is the smallest, and the precipitation rate of lithium carbonate in this step can be improved.
  • the third halogenation can cause the lithium loss caused by incomplete washing or extraction to be returned to the extraction process for cyclic extraction, so that the extraction rate of lithium ions in the brine reaches or approaches 100%.
  • the carbonate ion and the magnesium ion react exactly according to the chemical equation to determine the proportion of halogen (the same as when the first halogen is used, but the lithium recovery is completely solved). Rate problem, and there is no industrial wastewater discharge in the whole process, no environmental pollution).
  • the third halogenated liquid returned to the first halogenated system.
  • the liquid after the third halogenation can be divided into three cases of directly mixing with the first halogenated brine, first concentrating and mixing, and then concentrating and separating the solids.
  • the evaporation and concentration of the brine after the third halogenation including evaporation and concentration directly after mixing with the brine after the first halogenation, can make the content of lithium ions in the water more than 4 g/l, preferably the lithium ion concentration reaches 7.5 ⁇ 8.5 g / l, the specific requirements are the same as the first condensation requirements after halogenation.
  • the third halogenation process can be carried out at 0 to 90 ° C. For cost and other factors (such as solubility), it is usually at room temperature (20 to 30 ° C).
  • the invention provides a brine-type brine and a sulfate-type brine or a chloride-type magnesium-containing brine, which is firstly halogenated according to the composition of the brine, naturally concentrated and evaporated at room temperature, and then halogenated for the second time. Lithium carbonate is precipitated, and the liquid after the precipitation of lithium carbonate is returned to the previous process to re-halogenate, thereby forming a production method of overlapping lithium halide to produce lithium carbonate.
  • the present invention is directed to two problems in the process of extracting lithium from two types of water, and is proposed in conditional
  • the area that is, there are two or several places with two types of brine, the water body transfer according to the actual situation, because the composition or composition ratio of the brine in Cambodia salt lake is difficult to be the same, even if the same salt lake changes with the season, its composition changes It is also large, and even a few salt lakes have different types of brines. Therefore, when transferring water bodies, it is necessary to comprehensively consider the amount of water transfer, the direction of transfer, altitude (preferably self-flow), and the storage capacity of water-transfer salt lakes. Factors such as the area of the salt field.
  • the brine of two salt lakes or several salt lakes can be mixed and blended, and the unfavorable factors become favorable factors, that is, the sulfate type is removed by the co 3 2 -ion ions in the carbonate type brine.
  • the magnesium ion in the brine allows the separation of magnesium and lithium.
  • the use of magnesium ions in the sulphate-type brine removes the carbonate ions in the carbonate-type brine, which facilitates the enrichment of lithium and thus reaches the brine.
  • Lithium can be both enriched and extracted.
  • the first halogenation and the third halogenation are based on the above principles.
  • the second halogenation is the carbonate content in the carbonate-type brine (the lithium ion is close to or saturated) after evaporation, and the brine after the first halogenation is concentrated by evaporation, and the lithium ion is concentrated.
  • the amount of carbonate ions is 100 ⁇ 130% of the theoretical amount
  • the third halogenation is the content of Mg 2+ ions in the sulphate brine and the C0 3 2 content in the liquid after the second precipitation of lithium carbonate.
  • the magnesium ions react exactly with the carbonate ions.
  • Specific magnesium ion: carbonate 1: 2.469-2.470, the ratio of halogen is determined.
  • the brine only removes magnesium ions without lithium ion loss during the first blending.
  • the reason is that the basic magnesium carbonate formed is a poorly soluble compound.
  • the solubility of lithium carbonate is: 1.54 g (0 ° C), 1.33 g (20 ° C), 0.72 g (100 ° C).
  • the solubility of lithium carbonate is small.
  • the solubility of lithium carbonate is: 1.54g (0°C), 1.33g (20°C), 0.72g (100V), so the lithium carbonate-containing brine is evaporated when the brine is evaporated.
  • the lithium ion content in the brine can reach up to 1.5g/l, otherwise it will precipitate in the form of lithium carbonate.
  • the lithium ion content can reach 2.5g/l, so in the secondary halogen process, evaporation and concentration to lithium
  • the content of lithium ions in the ion-saturated or near-saturated carbonate-type brine is 1.5 to 2.5 g/l.
  • the basic magnesium carbonate in the present invention means 3MgCO 3 ⁇ Mg(0H) 2 ⁇ 4H 2 0 or MgCO 3 ⁇ Mg(0H) 2 .
  • Evaporative concentration in the present invention includes evaporative concentration in a natural (e.g., daylight) manner, as well as evaporation by artificial heating, artificial light, or other artificial means.
  • the solid-liquid separation in the present invention includes separating the solid or liquid therein by special equipment, and also directly performing precipitation separation in a salt field or other places or facilities, and also includes various filtrations. The steps or facilities are separated.
  • the invention basically does not need external raw materials, has low input, simple process, can be used for large-scale lithium carbonate production, has high acquisition rate, and the product quality reaches national standard, and is particularly suitable for Georgia salt lake (mixed layout of two types of salt lakes). Development of lithium resources.
  • the invention is suitable for the production of carbonate type (lithium-containing) salt lake brine and brine of any type (including magnesium, lithium) salt lake brine, thereby solving the carbonate type and sulfate type salt lake (lithium containing) brine in lithium salt
  • Two problems of lithium enrichment and separation of magnesium and lithium in the extraction process it has strong adaptability to raw materials, high acquisition rate and low cost. Because the production process relies on solar thermal energy to naturally evaporate brine, and no external raw materials and other chemistry are needed. The agent is the second time to remove lithium carbonate from the halogen, and it is carried out at room temperature in the factory. The lithium salt is washed with 80°C hot water. Because the dosage is small, solar water can be used, so the factory production is basically pollution-free.
  • the invention basically does not need external raw materials, has low input, simple process, can be used for large-scale lithium carbonate production, has high acquisition rate, and the product quality reaches national standard, and is particularly suitable for Georgia salt lake (mixed layout of two types of salt lakes). Development of lithium resources. DRAWINGS
  • Figure 1 is a process flow diagram of the present invention. detailed description
  • Yantian operations can be carried out after the completion of Yantian construction and the transfer of a certain type of water body to a salt field in another type of water body salt lake.
  • the carbonate type brine and the sulphate type brine are halogenated according to the process requirement ratio (CO/- and Mg 2+ ), and the brine completed by the halogen is concentrated by natural evaporation to enrich lithium ions (when lithium is concentrated to 3 g/1)
  • the saturation point of potassium ions will be reached, until the lithium ion in the brine is enriched to a certain content (the higher the Li+, the higher the precipitation rate of lithium carbonate), and it is used.
  • the lithium carbonate slurry is filtered, washed in countercurrent for more than three times, and dried to obtain a powdered lithium carbonate product.
  • each halogen operation is based on the inspection results of the brine composition at each stage. After calculating and determining the proportion of halogen in each stage, input the multi-point control industrial computer, and the computer will command each halogen flow meter device. For halogen operation, the flow and total amount of halogen should be accurate to ensure the accuracy of the ratio of halogen.
  • brine: brine 3.5: 1 (according to eight, 10% excess of carbonate ion in brine), take eight, 35 liters of brine, 10 liters of brine, with halogen under stirring, after the completion of halogen After stirring for another 4 hours, the stirring was stopped, and the mixture was allowed to stand for 2 hours, and the supernatant liquid was removed, and the lower layer slurry was filtered to obtain a cake and a clear liquid.
  • the amount of carbonate ions is 100 to 130% of the theoretical amount.
  • step 3 4.
  • the amount of clear liquid in step 3 is 44.6L, and its composition is:
  • the filter cake of the third step is backwashed with 8 (TC hot water) three times. After filtration, the filter cake is dried, and the dried product is a lithium carbonate product. After washing and drying, the lithium carbonate is 310g, and the purity is: 99.44%, and the single-line precipitation rate of lithium is 77.3% (refers to B t brine) minus three of the countercurrent washing loss lithium is about the total amount of finished lithium. 6%, The actual single-line acquisition rate was 72.4%.
  • the third halogenation that is, the carbonate ion in the clear liquid is reacted with the magnesium ion in the B lake brine to form basic carbonic acid.
  • the brine enters the brine system after the first halogenation, and continues to evaporate and concentrate to obtain lithium-enriched brine, which participates in the second halogenation, and completes the entire process of overlapping halogenation.
  • the total yield of lithium the leakage of brine in the natural evaporation of salt fields and the entrainment of other salts in the evaporation of salt fields are unavoidable in any salt field production, and usually do not affect the calculation of the total production rate of the workshop. According to the above routine, when the total yield of lithium in the process is calculated, in addition to the run, run, drip, and leak in the production workshop, the lithium salt is substantially completely recovered.
  • step 3 4. The amount of clear liquid in step 3 is 13.85L, and its composition is:
  • step 3 The filter cake of step 3 is backwashed with 80°C hot water three times. After filtration, the filter cake is dried and baked. The dry product is a lithium carbonate product.
  • the lithium carbonate After washing and drying, the lithium carbonate is 273g, and the purity is 99. 21%.
  • the single-line precipitation rate of lithium is 76.93% (referred to as brine) minus three of the countercurrent washing losses. Lithium is about 6% of the total amount of finished lithium. The actual single-line acquisition rate was 72.3%. 6.
  • D-halogen brine for halogenation which is called the third halogenation, that is, the carbonate ion in the clear liquid is reacted with the magnesium ion in the D lake brine to form basic carbonic acid.

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Abstract

L'invention concerne un procédé de production de carbonate de lithium par application d'un procédé d'ajout de plusieurs eaux mères et utilisation d'une eau mère de type carbonate et d'une eau mère de type sulfate (ou d'une eau mère contenant du magnésium) en tant que matières premières, qui comprend l'application de la première étape d'ajout d'eau mère par mélange d'une eau mère de type carbonate avec une eau mère de type sulfate, les ions CO3 2- et Mg2+ dans les eaux mères réagissant complètement les uns avec les autres pour produire du carbonate de magnésium basique, l'évaporation et la concentration des eaux mères, l'application d'une séparation solide-liquide pour éliminer le précipité de carbonate de magnésium basique et pour obtenir une eau mère enrichie en lithium ; l'application de la deuxième étape d'ajout d'eau mère par mélange de l'eau mère enrichie en lithium avec une eau mère de type carbonate qui est évaporée et concentrée à une concentration de saturation en ion lithium ou une concentration proche de la concentration de saturation en ion lithium, de manière à produire du carbonate de lithium par l'ion Li+ contenu dans l'eau mère mélangée, l'application d'une séparation solide-liquide pour éliminer le précipité de carbonate de lithium, le lavage du précipité de carbonate de lithium obtenu avec de l'eau chaude, le séchage, puis l'obtention d'un produit carbonate de lithium. Le procédé est simple, les matières premières peuvent facilement être obtenues et le rendement est élevé.
PCT/CN2011/082081 2011-10-14 2011-11-11 Procédé de production de carbonate de lithium par application d'un procédé d'ajout de plusieurs eaux mères et utilisation d'une eau mère de type carbonate et d'une eau mère de type sulfate en tant que matières premières Ceased WO2013053165A1 (fr)

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CN1454843A (zh) * 2003-03-21 2003-11-12 钟辉 一种硫酸镁亚型盐湖卤水镁锂分离方法

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CN105905929A (zh) * 2016-04-07 2016-08-31 中国科学院青海盐湖研究所 从高原碳酸盐型卤水中制备碳酸锂的方法
CN113493216A (zh) * 2021-07-12 2021-10-12 青海锂业有限公司 一种盐湖卤水制备电池正极材料行业级碱式碳酸镁的方法

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