CN115920450A - Auxiliary extraction agent for extracting boric acid from salt lake brine and method for extracting boric acid - Google Patents
Auxiliary extraction agent for extracting boric acid from salt lake brine and method for extracting boric acid Download PDFInfo
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Abstract
The invention discloses an ionic liquid auxiliary extraction agent for extracting boric acid from salt lake brine and a method for extracting boric acid from salt lake brine by using the ionic liquid as the auxiliary extraction agent. The ionic liquid reinforced extraction agent has the characteristics of good selectivity, high efficiency, low cost and the like in extracting boron from salt lake brine, and has wide application prospect. The extraction aid can enhance the extraction effect of the process of extracting boric acid from salt lake brine and improve the single-stage extraction efficiency.
Description
Technical Field
The invention belongs to the technical field of salt lake chemical industry, and particularly relates to an auxiliary extracting agent for extracting boric acid from salt lake brine and a method for extracting boric acid.
Background
The boron resource reserves in Qinghai province are abundant, the boron resource reserves are second in China, and the large ore deposits mainly comprise large chai dan lakes, small Chai Dan lakes, yiliping, west tai Ji Naier, and salt lakes such as Keerfeng. Boric acid is an industrial boride with a very wide range of applications. Boric acid is mainly used in the glass making industry, in the enamel and ceramic industries to enhance the gloss and fastness of articles. Boron steel made by doping boron in the steel industry has higher hardness and good rolling ductility, and can replace nickel steel. Can be used as bactericide in medicine. In addition, it can be used as a preservative for wood. Used as boron fertilizer in agriculture. It is also widely used in the manufacture of metal welding, leather, capacitor, plating, cosmetics, etc. Boric acid is a main raw material for producing various boron compounds. The solid boron ore resources in Qinghai province are exhausted basically after being mined for decades, and a large amount of boron is produced as a byproduct in the process of extracting lithium from salt lake brine, so that the solid boron ore resources cannot be industrially utilized all the time.
The west station Ji Naier salt lake is characterized by being rich in potassium, boron and lithium, and found that the amount of lithium resources (in terms of lithium chloride) was 263 ten thousand tons, the amount of potassium resources (in terms of potassium chloride) was 2073 ten thousand tons, and the amount of boron resources (in terms of diboron trioxide) was 155 ten thousand tons. The efficient development and utilization of the lithium, potassium and boron resources can improve the comprehensive utilization benefits of the salt lake and is a powerful component for creating a world-level salt lake industrial base by the Qinghai. The national security science and technology development company of Qinghai China starts to carry out the operation of acidizing the old brine to prepare the boric acid in 2016 (4 months), and the crude boric acid is produced in 2017 (about 2.5 ten thousand tons) all the year round, B 2 O 3 The average grade is 18.6 percent, the impurity content is high, and about 4000 tons of refined boric acid products can be produced by adopting a hot-melt cold crystallization process. Although partial boric acid refining is realized, the process and equipment are limited, and the quality of refined boric acid products cannot be effectively improved.
The demand of modern industry for boron is increasing, and the mature and efficient development technology of boron is significant. Boron is mainly distributed in solid ores and liquid ores, along with the massive exploitation of the boron ores, the boron in the solid ores is almost exhausted, and the development of a mature and efficient technology for extracting the boron in the liquid ores is very important. The research of developing and utilizing boron resources in salt lake brine in China is still in the primary stage. The continuous development and utilization of boron mineral resources and the immature technology thereof lead to the reduction of high-quality boron resources in China and also cause the waste of resources and the pollution of salt lake environment, so that how to utilize the boron resources in a green and efficient manner, especially how to extract the boron resources from salt lake brine, is becoming more and more urgent.
At present, the technology for extracting boron from salt lake brine mainly comprises an acidification crystallization method, a precipitation method, a flotation method, an ion exchange method, a solvent extraction method and the like. The extraction rate of boron by the acidification crystallization method is only 50-60%, and the acidification crystallization method is only suitable for raw material brine with high boron content; the precipitation method consumes a large amount of acid; the ion exchange method is limited in industrial production by process and cost. The solvent extraction method is less limited by the boric acid content in the solution, and has the advantages of short process flow, simple production equipment and simple and convenient operation, thus being an ideal boron extraction method with wide application prospect. But the adopted monohydric alcohol extractant has the problems of low single-stage extraction rate, multiple required extraction stages and the like; thus causing great loss of solvent, causing pollution to the water phase after the lost extractant enters the water phase, and improving the extraction rate of a single stage is a very important problem to be solved. The glycol extractant has poor viscosity, high loss rate and poor oil solubility, and limits industrial application to a certain extent.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides an ionic liquid co-extractant for extracting boric acid from salt lake brine and a method for extracting boric acid from salt lake brine by using the ionic liquid as the co-extractant. The ionic liquid reinforced extraction agent has the characteristics of good selectivity, high efficiency, low cost and the like in extracting boron from salt lake brine, and has wide application prospect. The extraction aid can enhance the extraction effect of the process of extracting boric acid from salt lake brine and improve the single-stage extraction efficiency.
The invention is realized by the following technical scheme:
an auxiliary extractant for extracting boric acid from salt lake brine, wherein the auxiliary extractant is an ionic liquid, and anions in the ionic liquid include but are not limited to chloride ions, acetate ions, hydrogen phosphate ions, dihydrogen phosphate ions, sulfate ions, hydrogen sulfate ions, carbonate ions, bicarbonate ions, methylsulfonate ions, trifluoromethylsulfonate ions and the like;
the cations of the ionic liquid extraction aid are 3-methylimidazole cations with different side chain lengths, pyridine cations with different side chain lengths and the like; the structural formula of the compound is shown as follows,
wherein: r 1 And R 2 Are all C 11 ～C 20 A linear alkyl group of (1).
In the technical scheme, the anion of the ionic liquid is hydrogen sulfate radical ion and methylsulfonate radical ion;
r of cation of the ionic liquid 1 And R 2 Is C 12 ～C 16 Linear alkyl group of (1).
A method for extracting boric acid from salt lake brine adopts the extraction aid for extracting boric acid from salt lake brine in the technical scheme.
Research shows that when the anion of the ionic liquid is methylsulfonate ion and the cation is cation in a preferred range, the single-stage extraction rate of the boric acid can be remarkably improved to 90-95% from 54% of that of the extraction aid-free extraction agent; when the anion of the ionic liquid is bisulfate ion and the cation is the cation in the preferred range, the single-stage extraction rate of the boric acid can be remarkably improved to 92-95 percent.
A method for extracting boric acid from salt lake brine by using ionic liquid in the technical scheme as an extraction aid comprises the following steps:
step 1, mixing the extraction aid, the extractant and the diluent to obtain an extracted organic phase; the volume ratio of the extracting agent to the diluting agent is 1: 0.25-1.5; preferably 1 to (0.6-1);
the addition amount of the extraction assistant agent relative to the extraction agent is 1 g/(30-60) mL, preferably 1 g/(40-50) mL;
mixing and extracting the extracted organic phase and acidified salt lake brine, and obtaining a boric acid loaded organic phase and raffinate water after phase splitting;
step 2, mixing the boric acid loaded organic phase with a stripping agent, carrying out back extraction, and carrying out phase separation to obtain a water phase containing boric acid and an organic phase poor in boric acid;
the back extraction agent is a neutral or weakly acidic aqueous solution.
In the technical scheme, the extracting agent is monohydric aliphatic alcohol and/or dihydric aliphatic alcohol;
the monohydric aliphatic alcohol is preferably at least one of isoamyl alcohol and isooctyl alcohol;
the dihydric fatty alcohol is preferably at least one of 1,2-dihydric alcohol and 1,3-dihydric alcohol.
In the technical scheme, the diluent is a diluent with the kinematic viscosity of not higher than 8mm at 20 DEG C 2 Hydrophobic organic solvent/s, preferably aviation kerosene.
In the technical scheme, the pH value of the acidified salt lake brine is 2-3, and preferably 2-2.6;
the process of acidifying the salt lake brine adopts hydrochloric acid for acidification.
In the technical scheme, in the process of mixing and extracting the extraction organic phase and the acidified salt lake brine, the volume ratio of the extraction organic phase to the acidified salt lake brine is preferably 1: 1-1.2.
In the technical scheme, in the process of mixing and extracting the extracted organic phase and the acidified salt lake brine, the extraction temperature is 20-40 ℃, and the preferable temperature is 20-25 ℃; the extraction time is preferably 20 to 30min.
In the technical scheme, the pH value of the stripping agent is 6-7; preferably the stripping agent is deionized water.
In the above technical scheme, in the process of mixing the boric acid loaded organic phase with the stripping agent for stripping, the volume ratio of the stripping agent to the boric acid loaded organic phase is preferably 1: 1-1.2.
In the technical scheme, in the back extraction process by mixing the boric acid loaded organic phase and the stripping agent, the back extraction temperature is 20-40 ℃, preferably 20-25 ℃, and the back extraction time is preferably 20-30 min.
The invention has the advantages and beneficial effects that:
the key point of solvent extraction is the selection of an extraction system, so that aiming at different types of salt lakes, the optimization of the extraction system with good extraction performance and low water solubility is the hot spot of current research. The basic mechanism of the method for extracting boric acid from salt lake brine is as follows (the extracting agent is isooctyl alcohol as an example):
the acidified salt lake brine and isooctyl alcohol are subjected to esterification reaction to generate monoisooctyl borate, diisooctyl borate and triisooctyl borate (hereinafter referred to as boric acid ester); these esters have very little solubility in water but have better solubility in the organic phase, allowing boric acid to be extracted into the organic phase as borate esters.
(II) under the acidic condition, the borate ester is easy to generate hydrolysis reaction, and the hydrolysis process is generally carried out in two steps: the first hydrolysis step produces hydrogen ions and borate anions, followed by further hydrolysis to produce boric acid and isooctanol.
And (III) micelles formed by the ionic liquid (the extraction aid) dissolved in the organic phase selectively extract the borate formed at the phase interface, so that the diffusion of the borate is accelerated, and the aim of enhancing the extraction of the boric acid is fulfilled.
The content of ions contained in different types of salt lake brine may not be the same or similar, but other ions have no obvious influence on the system, so that the extraction system disclosed by the application can be applied to all boron-containing salt lake brine instead of only one type of salt lake brine in the application process.
In the technical scheme of the invention, the cation structural formulas (I) and (II) of the ionic liquid extraction aid are hydrophobic cations and both contain N atoms, and the N atoms can form hydrogen bonds with complex boric acid ester, so that the technical effect of selective extraction is achieved.
Compared with the prior art, the method for extracting boric acid from salt lake brine has the following beneficial effects:
1. the invention provides a novel method for extracting boric acid, which takes ionic liquid as an extraction aid and is used for extracting boric acid from salt lake brine, and can greatly improve the single-stage extraction rate of boric acid;
2. the ionic liquid extraction aid provided by the invention can obviously increase the single-stage extraction rate of boric acid from 54% without the extraction aid to 90-95%;
3. the cation alkyl chain carbon number of the ionic liquid extraction aid provided by the invention is greater than 10, the ionic liquid extraction aid is insoluble in water, the extraction aid cannot be lost in the extraction process, and the quality of boric acid products cannot be influenced in the back extraction process;
4. the method for extracting the boric acid has simple production equipment in the actual production process, is simple and convenient to operate, and can realize high-value recovery of the boron extracted from the salt lake brine.
Detailed Description
In order to make the technical field of the invention better understand, the technical scheme of the method for extracting the boric acid from the salt lake brine is further described by combining the specific examples.
The pH value of the Qinghai salt lake brine used in each experiment of the invention is 4.2, the Qinghai salt lake brine contains 28.5g/L of boric acid, and the main components are shown in Table 1.
TABLE 1 Main composition of Qinghai salt lake brine
| Composition (I) | H 3 BO 3 | Mg 2+ | Li + | SO 4 2- | Cl - |
| content/g.L -1 | 28.5 | 109.9 | 1.9 | 27 | 287.4 |
Example one
Acidifying 20mL of Qinghai salt lake brine by using 2mol/L hydrochloric acid to adjust the pH value to 2.6, thereby obtaining acidified salt lake brine;
adopting 10mL of isooctanol as an extracting agent and 10mL of aviation kerosene as a diluting agent, fully mixing the isooctanol and the aviation kerosene, and dissolving 0.25g of 1-dodecyl-3-methylimidazole hydrogen sulfate as an auxiliary extracting agent in the mixed solution in an ultrasonic oscillation mode to form an extracted organic phase;
mixing the acidified salt lake brine with the extraction organic phase, performing water bath constant-temperature oscillation extraction at 20 ℃, standing for layering to obtain an extraction organic phase containing borate anions, wherein the extraction time is 20 min; the extraction rate was determined to be 92.6%.
And (3) performing water bath constant-temperature oscillation back extraction at 20 ℃ by using 20mL of deionized water as a back extraction agent for 20min, and standing for layering to obtain an aqueous solution containing boric acid. The back extraction rate was calculated to be 74.0% by measurement.
Example two
Acidifying 20mL of Qinghai salt lake brine by using 2mol/L hydrochloric acid to adjust the pH value to 2.6, thereby obtaining acidified salt lake brine;
adopting 10mL of isooctanol as an extracting agent and 10mL of aviation kerosene as a diluting agent, fully mixing the isooctanol and the aviation kerosene, and dissolving 0.25g of 1-dodecyl-3-methylimidazol methyl sulfonate as an auxiliary extracting agent in the mixed solution in an ultrasonic oscillation mode to form an extracted organic phase;
mixing the acidified salt lake brine with the extraction organic phase, performing water bath constant-temperature oscillation extraction at 20 ℃, standing for layering to obtain an extraction organic phase containing borate anions, wherein the extraction time is 20 min; the extraction rate is 90.0% by measurement calculation.
And (2) adopting 20mL of deionized water as a back extraction agent, carrying out water bath constant-temperature oscillation back extraction at 20 ℃, wherein the back extraction time is 20min, and standing for layering to obtain an aqueous solution containing boric acid. The back extraction rate was calculated to be 72.4% by measurement.
EXAMPLE III
Acidifying 20mL of Qinghai salt lake brine by using 2mol/L hydrochloric acid to adjust the pH value to 2.6, thereby obtaining acidified salt lake brine;
adopting 12mL of isooctanol as an extracting agent and 8mL of aviation kerosene as a diluting agent, fully mixing the isooctanol and the aviation kerosene, and dissolving 0.25g of 1-tetradecyl-3-methylimidazole bisulfate as an auxiliary extracting agent in the mixed solution in an ultrasonic oscillation mode to form an extraction organic phase;
mixing the acidified salt lake brine with the extracted organic phase, performing water bath constant-temperature oscillation extraction at 20 ℃, standing for 20min, and layering to obtain an extracted organic phase containing borate anions; the extraction rate was determined to be 93.5%.
And (3) performing water bath constant-temperature oscillation back extraction at 20 ℃ by using 20mL of deionized water as a back extraction agent for 20min, and standing for layering to obtain an aqueous solution containing boric acid. The back extraction rate is calculated to be 76.2% through measurement.
Example four
Acidifying 20mL of Qinghai salt lake brine by using 2mol/L hydrochloric acid to adjust the pH value to 2.6, thereby obtaining acidified salt lake brine;
adopting 12mL of isooctanol as an extracting agent and 8mL of aviation kerosene as a diluting agent, fully mixing the two, and dissolving 0.25g of 1-tetradecyl pyridine bisulfate as an auxiliary extracting agent in the mixed solution in an ultrasonic oscillation mode to form an extracted organic phase;
mixing the acidified salt lake brine with the extraction organic phase, performing water bath constant-temperature oscillation extraction at 20 ℃, standing for layering to obtain an extraction organic phase containing borate anions, wherein the extraction time is 20 min; the extraction rate is 94.7% by measurement calculation.
And (3) performing water bath constant-temperature oscillation back extraction at 20 ℃ by using 20mL of deionized water as a back extraction agent for 20min, and standing for layering to obtain an aqueous solution containing boric acid. The back extraction rate was determined to be 78.0%.
EXAMPLE five
Acidifying 20mL of Qinghai salt lake brine by using 2mol/L hydrochloric acid to adjust the pH value to 2.6 to obtain acidified salt lake brine;
adopting 11mL of isooctanol as an extracting agent and 9mL of aviation kerosene as a diluting agent, fully mixing the two, and dissolving 0.25g of 1-hexadecyl pyridine bisulfate as an auxiliary extracting agent in the mixed solution in an ultrasonic oscillation mode to form an extracted organic phase;
mixing the acidified salt lake brine with the extraction organic phase, performing water bath constant-temperature oscillation extraction at 20 ℃, standing for layering to obtain an extraction organic phase containing borate anions, wherein the extraction time is 20 min; the extraction rate was calculated by measurement to be 93.9%.
And (3) performing water bath constant-temperature oscillation back extraction at 20 ℃ by using 20mL of deionized water as a back extraction agent for 20min, and standing for layering to obtain an aqueous solution containing boric acid. The back extraction rate is calculated to be 76.9% through measurement.
EXAMPLE six
Acidifying 20mL of Qinghai salt lake brine by using 2mol/L hydrochloric acid to adjust the pH value to 2.6 to obtain acidified salt lake brine;
adopting 11mL of isooctanol as an extracting agent and 9mL of aviation kerosene as a diluting agent, fully mixing the two, and dissolving 0.25g of 1-hexadecyl pyridine methyl sulfonate as an auxiliary extracting agent in the mixed solution in an ultrasonic oscillation mode to form an extracted organic phase;
mixing the acidified salt lake brine with the extraction organic phase, performing water bath constant-temperature oscillation extraction at 20 ℃, standing for layering to obtain an extraction organic phase containing borate anions, wherein the extraction time is 20 min; the extraction rate was determined to be 92.2%.
And (3) performing water bath constant-temperature oscillation back extraction at 20 ℃ by using 20mL of deionized water as a back extraction agent for 20min, and standing for layering to obtain an aqueous solution containing boric acid. The back extraction rate was determined to be 73.6%.
Comparative example
Compared with the first embodiment, the method is only different in that no ionic liquid co-extractant is added in the extraction process.
Acidifying 20mL of Qinghai salt lake brine by using 2mol/L hydrochloric acid to adjust the pH value to 2.6, thereby obtaining acidified salt lake brine;
adopting 10mL of isooctanol as an extracting agent and 10mL of aviation kerosene as a diluent, and fully mixing the two by an ultrasonic oscillation mode to form an extracted organic phase;
mixing the acidified salt lake brine with the extraction organic phase, performing water bath constant-temperature oscillation extraction at 20 ℃, standing for layering to obtain an extraction organic phase containing borate anions, wherein the extraction time is 20 min; the extraction rate was found to be 54.0% by measurement.
And (3) performing water bath constant-temperature oscillation back extraction at 20 ℃ by using 20mL of deionized water as a back extraction agent for 20min, and standing for layering to obtain an aqueous solution containing boric acid. The back extraction rate was calculated by measurement to be 78.0%.
Both dihydric alcohol and monohydric alcohol contain hydroxyl structures, and both the dihydric alcohol and the monohydric alcohol are subjected to esterification reaction with boric acid to generate ester, and then are extracted, so both monohydric aliphatic alcohol and dihydric aliphatic alcohol can be used, and the dihydric alcohol is higher in cost, so that the dihydric alcohol is not used as an example in a specific embodiment.
The invention being thus described by way of example, it should be understood that any simple alterations, modifications or other equivalent alterations as would be within the skill of the art without the exercise of inventive faculty, are within the scope of the invention.
Claims (10)
1. An auxiliary extraction agent for extracting boric acid from salt lake brine, which is characterized in that the auxiliary extraction agent is an ionic liquid, and anions in the ionic liquid include but are not limited to chloride ions, acetate ions, hydrogen phosphate ions, dihydrogen phosphate ions, sulfate ions, hydrogen sulfate ions, carbonate ions, hydrogen carbonate ions, methylsulfonate ions, trifluoromethylsulfonate ions and the like;
the positive ions of the ionic liquid extraction aid are 3-methylimidazole positive ions with different side chain lengths, pyridinium positive ions with different side chain lengths and the like; the structural formula of the compound is shown as the formula,
wherein: r 1 And R 2 Are all C 11 ～C 20 Linear alkyl group of (1).
2. An extraction aid according to claim 1 wherein the anion of the ionic liquid is a bisulfate ion and a methylsulfonate ion;
r of cation of the ionic liquid 1 And R 2 Is C 12 ～C 16 Linear alkyl group of (1).
3. A method for extracting boric acid from salt lake brine, which is characterized in that the auxiliary extractant used for extracting boric acid from salt lake brine as claimed in claim 1 or 2 is used.
4. A method for extracting boric acid from salt lake brine, which is characterized in that the auxiliary extractant for extracting boric acid from salt lake brine, which is disclosed by claim 1 or 2, is adopted, and comprises the following steps:
step 1, mixing the extraction aid, the extractant and the diluent to obtain an extracted organic phase; the volume ratio of the extracting agent to the diluting agent is 1: 0.25-1.5; preferably 1 to (0.6-1);
the addition amount of the auxiliary extraction agent relative to the extraction agent is 1 g/(30-60) mL, preferably 1 g/(40-50) mL;
mixing and extracting the extracted organic phase and acidified salt lake brine, and obtaining a boric acid loaded organic phase and raffinate water after phase splitting;
step 2, mixing the boric acid loaded organic phase with a stripping agent, carrying out back extraction, and carrying out phase separation to obtain a water phase containing boric acid and an organic poor phase;
the stripping agent is a neutral or weakly acidic aqueous solution.
5. The method for extracting boric acid from salt lake brine as claimed in claim 4, wherein the extractant is a monohydric aliphatic alcohol and/or a dihydric aliphatic alcohol;
the monohydric aliphatic alcohol is preferably at least one of isoamyl alcohol and isooctyl alcohol;
the dihydric fatty alcohol is preferably at least one of 1,2-dihydric alcohol and 1,3-dihydric alcohol.
6. The method of claim 4, wherein the diluent is a solvent having a kinematic viscosity of not greater than 8mm at 20 ℃ 2 A hydrophobic organic solvent per second, preferably jet fuel.
7. The method for extracting boric acid from salt lake brine according to claim 4, wherein the pH value of the acidified salt lake brine is 2-3, preferably 2-2.6;
the process of acidifying the salt lake brine adopts hydrochloric acid for acidification.
8. The method of claim 4, wherein the volume ratio of the organic phase to the acidified salt lake brine is 1: 1-1.2 during the mixing and extraction of the organic phase with the acidified salt lake brine.
9. The method for extracting boric acid from salt lake brine according to claim 4, wherein the extraction temperature is 20-40 ℃, preferably 20-25 ℃ in the process of mixing and extracting the extraction organic phase and the acidified salt lake brine; the extraction time is preferably 20 to 30min.
10. The method for extracting boric acid from salt lake brine according to claim 4, wherein the stripping agent has a pH value of 6 to 7; preferably, the stripping agent is deionized water;
in the process of mixing the boric acid loaded organic phase with a stripping agent for stripping, the volume ratio of the stripping agent to the boric acid loaded organic phase is preferably 1: 1-1.2;
and in the process of mixing the boric acid loaded organic phase with a stripping agent for stripping, the stripping temperature is 20-40 ℃, preferably 20-25 ℃, and the stripping time is preferably 20-30 min.
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| CN117244402A (en) * | 2023-11-17 | 2023-12-19 | 西安稀有金属材料研究院有限公司 | Method for extracting and separating boron isotopes |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117244402A (en) * | 2023-11-17 | 2023-12-19 | 西安稀有金属材料研究院有限公司 | Method for extracting and separating boron isotopes |
| CN117244402B (en) * | 2023-11-17 | 2024-02-09 | 西安稀有金属材料研究院有限公司 | Method for extracting and separating boron isotopes |
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