CN101544378A - Process method for extracting low-concentration boracic acid in magnesium-containing brine - Google Patents
Process method for extracting low-concentration boracic acid in magnesium-containing brine Download PDFInfo
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- CN101544378A CN101544378A CN200910068353A CN200910068353A CN101544378A CN 101544378 A CN101544378 A CN 101544378A CN 200910068353 A CN200910068353 A CN 200910068353A CN 200910068353 A CN200910068353 A CN 200910068353A CN 101544378 A CN101544378 A CN 101544378A
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Abstract
The invention relates to a process method for extracting low-concentration boracic acid in magnesium-containing brine, which comprises the following steps that: at room temperature, a mixed solvent mixed by monacid alcohol and a nonpolar organic solvent is used as a complexing extractant to extract acidified brine to obtain an extraction phase; then water is used for carrying out back extraction on the extraction phase; the boracic acid is back-extracted to a water phase; a mixed extraction solvent is regenerated; and the water phase containing the boracic acid is condensed and evaporated to directly obtain a boracic acid product. The process method can remove the low-content boron to substantially improve the quality of a produced magnesium product, can obtain the boracic acid as a byproduct, fully realizes the comprehensive development and utilization of magnesium-containing saline brine and has remarkable economic benefits.
Description
Technical field
The present invention relates to salt lake brine development of resources and comprehensive utilization process technology, lower concentration boric acid process for extracting in particularly a kind of magnesium-containing brine can be applicable to the extraction of magnesium-containing brine mesoboric acid.
Background technology
In the comprehensive development and utilization of salt lake brine, the chloride type bittern that contains potassium, magnesium, boron, after removing potassium, concentrate the heavy boron of acidifying, most of boron is separated out with the form of boric acid, the magnesium chloride aqueous salt brine of remaining low levels boron (about 8 grams per liters), this part aqueous salt brine can be used to produce and contain magnesium products, as magnesium chloride, magnesium oxide etc.But, have a strong impact on the magnesium products quality of production owing to the existence of low levels boron.
Chinese patent CN 200510085830.X discloses the technology of producing boric acid from borated water chloromagnesite saturated solution, it is raw material that this patent of invention has been introduced with borated water chloromagnesite saturated solution, puies forward the technology of boron, thick boric acid washing, dry four operations production of boric acid boric acid through bittern pre-treatment, acidifying.But bittern is acidified carry after, still exist the boric acid about 8g/l not to be extracted in the mother liquor, this part boric acid is having a strong impact on the quality of subsequent product.
Summary of the invention
The object of the present invention is to provide lower concentration boric acid process for extracting in a kind of magnesium-containing brine, can overcome the defective of prior art.Adopt processing method of the present invention, can remove this part low levels boron, the magnesium products quality of production is greatly enhanced, and can obtains byproduct boric acid, realize containing the comprehensive development and utilization of magnesium salts lake bittern water fully, remarkable in economical benefits.
The step that lower concentration boric acid process for extracting comprises in the magnesium-containing brine provided by the invention: under the room temperature, the bittern of the mixed solvent that mixes with monohydroxy-alcohol and non-polar organic solvent after as complexing extractant extraction acidifying, obtain extraction phase, water is stripped to extraction phase again, boric acid is stripped into aqueous phase, the hybrid extraction solvent reclamation, borated water carries out concentration and evaporation, directly obtains the boric acid product.
The step that lower concentration boric acid process for extracting comprises in the magnesium-containing brine provided by the invention:
1) under the room temperature, regulates between the brine ph, 0.1～4 with acid.
2) preparation C
4～10Monohydroxy-alcohol and the mixed solvent that mixes of non-polar organic solvent as complexing extractant.
3) with the bittern after the complexing extractant extraction acidifying, the volume ratio of complexing extractant and bittern is 0.1～10:1, and the boric acid in the bittern is extracted in the extraction phase, obtains extraction phase, boron content in the bittern of extraction back is reduced to below 30 mg/litre, no longer influences the magnesium products quality.
4) water is to the extraction phase regeneration of stripping, and the volume ratio of water and extraction phase is 0.1～10:1, and boric acid is stripped into aqueous phase, and extraction agent obtains regeneration, can be recycled.
5) borated water is carried out concentration and evaporation, directly obtain the boric acid product.
Described acid is hydrochloric acid, and described monohydroxy-alcohol is butanols, Virahol, isopropylcarbinol, amylalcohol, hexanol, enanthol, octanol and decyl alcohol.The volume fraction of alcohol is 0.1～0.99.
Described non-polar organic solvent is benzene,toluene,xylene, solvent oil, kerosene etc.
Outstanding technical characterstic of the present invention is: the complexing extractant of using preparation, adopt method of extraction, removed the boric acid that contains in the magnesium boron bittern, the magnesium products quality of producing is greatly enhanced, simultaneously with the pure water back extraction complexing extractant of having regenerated, extraction agent is recycled, obtained byproduct boric acid.
Lower concentration boric acid process for extracting can overcome the defective of prior art in the magnesium-containing brine provided by the invention, compares with prior art absorption method and ion exchange method, and production cost is low, and the type selecting of production unit is easy.Adopt extraction process in addition, equipment and process design method maturation realize industrialization easily.Realize containing the comprehensive development and utilization of magnesium salts lake bittern water fully, remarkable in economical benefits.
Embodiment.
Describe processing step of the present invention and result in conjunction with the embodiments in detail.
Embodiment 1
Test sample of the present invention is the bittern behind the heavy boron of the bittern acidifying in West Platform salt lake, Qinghai, and composition is composed as follows:
Grams per liter B
2O
3Mg
2+Cl
-SO
4 2-
(concentration) 8.002 96.268 352.64 6.22
Processing step is as follows:
(1) under the room temperature, add concentrated hydrochloric acid in aqueous salt brine, regulating brine ph, is 3;
(2) hexanol is mixed with benzene, determining alcohol is 0.66, is made into complexing extractant.
(3) adopt the complexing extractant of preparing, than 2:1, bittern is carried out extraction process according to extraction phase.
(4) to the extraction phase regeneration of stripping, pure water: extraction phase=2:1.
(5) water that back extraction is obtained carries out solar evaporation, directly obtains the boric acid product.
Extraction back bittern boron content (mg/litre)=25 mg/litre
Reextraction organic phase boron content (mg/litre)=10 mg/litre.
Embodiment 2-4, experimental procedure the results are shown in Table 1 with embodiment 1.
Table 1: processing condition of the present invention and result
| Project | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Brine ph, | 0.1 | 1.5 | 4 |
| Adopt extraction agent | Butanols/toluene | Enanthol/No. 200 solvent oil | Decyl alcohol/kerosene |
| Determining alcohol (volume fraction) | 0.99 | 0.5 | 0.1 |
| The extraction phase ratio | 0.1：1 | 5∶1 | 10∶1 |
| Water is stripped and is compared | 0.1∶1 | 5∶1 | 10∶1 |
| Extraction back bittern boron content (mg/litre) | 26 | 20 | 22 |
| Reextraction organic phase boron content (mg/litre) | 8 | 5 | 4 |
Boron content in the bittern of extraction back is reduced to below 30 mg/litre as can be seen from Table 1, no longer influences the magnesium products quality.
Claims (8)
1, lower concentration boric acid process for extracting in a kind of magnesium-containing brine, it is characterized in that the step that comprises: under the room temperature, the bittern of the mixed solvent that mixes with monohydroxy-alcohol and non-polar organic solvent after as complexing extractant extraction acidifying, obtain extraction phase, water is stripped to extraction phase again, and boric acid is stripped into aqueous phase, the hybrid extraction solvent reclamation, borated water carries out concentration and evaporation, directly obtains the boric acid product.
2, lower concentration boric acid process for extracting in a kind of magnesium-containing brine is characterized in that the step that comprises:
1) under the room temperature, regulates between the brine ph, 0.1～4 with acid;
2) preparation C
4～10Monohydroxy-alcohol and the mixed solvent that mixes of non-polar organic solvent as complexing extractant;
3) with the bittern after the complexing extractant extraction acidifying, obtain extraction phase;
4) water is to the extraction phase regeneration of stripping, and boric acid is stripped into aqueous phase, and extraction agent obtains regeneration;
5) borated water is carried out concentration and evaporation, directly obtain the boric acid product.
3, process for extracting according to claim 2 is characterized in that described acid is hydrochloric acid.
4, process for extracting according to claim 2 is characterized in that described monohydroxy-alcohol is butanols, Virahol, isopropylcarbinol, amylalcohol, hexanol, enanthol, octanol or decyl alcohol.
5, according to claim 2 or 4 described process for extracting, the volume fraction that it is characterized in that described alcohol is 0.1～0.99.
6, process for extracting according to claim 2 is characterized in that described non-polar organic solvent is benzene,toluene,xylene, solvent oil or kerosene.
7, process for extracting according to claim 2, the volume ratio that it is characterized in that described complexing extractant and bittern is 0.1～10:1.
8, process for extracting according to claim 2, the volume ratio that it is characterized in that described water and extraction phase is 0.1～10:1.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102602953A (en) * | 2012-04-12 | 2012-07-25 | 青海锂业有限公司 | Method for preparing high borosilicate glass industry-level boric acid by utilizing salt lake lithium-extracting mother solution |
| CN103031448A (en) * | 2012-12-04 | 2013-04-10 | 中国科学院过程工程研究所 | Method for preenriching and separating lithium and boron from salt lake brine by liquid-liquid-liquid three-phase extraction |
| CN103482640A (en) * | 2013-09-27 | 2014-01-01 | 中国科学院青海盐湖研究所 | Method for separating boron from boron-containing bittern |
| CN103482643A (en) * | 2013-09-27 | 2014-01-01 | 中国科学院青海盐湖研究所 | Method for separating boron from bittern containing boron |
| CN103482642A (en) * | 2013-09-27 | 2014-01-01 | 中国科学院青海盐湖研究所 | Method for separating boron from bittern containing boron |
| CN103482641A (en) * | 2013-09-27 | 2014-01-01 | 中国科学院青海盐湖研究所 | Method for separating boron from boron-containing bittern |
| CN105347352A (en) * | 2015-12-09 | 2016-02-24 | 李洪岭 | High-efficiency and energy-saving new process for producing boric acid through heat reverse extraction method |
| CN108017067A (en) * | 2017-12-08 | 2018-05-11 | 中国科学院青海盐湖研究所 | The extraction system and its extracting process of boric acid are extracted from lake bittern water containing magnesium salts |
| CN109126200A (en) * | 2018-08-30 | 2019-01-04 | 山东省医学科学院药物研究所（山东省抗衰老研究中心、山东省新技术制药研究所） | The method of boric acid is extracted from the old halogen of high magnesium and mentions boron extractant |
-
2009
- 2009-04-03 CN CN2009100683534A patent/CN101544378B/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102602953A (en) * | 2012-04-12 | 2012-07-25 | 青海锂业有限公司 | Method for preparing high borosilicate glass industry-level boric acid by utilizing salt lake lithium-extracting mother solution |
| CN102602953B (en) * | 2012-04-12 | 2013-07-31 | 青海锂业有限公司 | Method for preparing high borosilicate glass industry-level boric acid by utilizing salt lake lithium-extracting mother solution |
| CN103031448A (en) * | 2012-12-04 | 2013-04-10 | 中国科学院过程工程研究所 | Method for preenriching and separating lithium and boron from salt lake brine by liquid-liquid-liquid three-phase extraction |
| CN103031448B (en) * | 2012-12-04 | 2014-07-30 | 中国科学院过程工程研究所 | Method for preenriching and separating lithium and boron from salt lake brine by liquid-liquid-liquid three-phase extraction |
| CN103482640A (en) * | 2013-09-27 | 2014-01-01 | 中国科学院青海盐湖研究所 | Method for separating boron from boron-containing bittern |
| CN103482643A (en) * | 2013-09-27 | 2014-01-01 | 中国科学院青海盐湖研究所 | Method for separating boron from bittern containing boron |
| CN103482642A (en) * | 2013-09-27 | 2014-01-01 | 中国科学院青海盐湖研究所 | Method for separating boron from bittern containing boron |
| CN103482641A (en) * | 2013-09-27 | 2014-01-01 | 中国科学院青海盐湖研究所 | Method for separating boron from boron-containing bittern |
| CN105347352A (en) * | 2015-12-09 | 2016-02-24 | 李洪岭 | High-efficiency and energy-saving new process for producing boric acid through heat reverse extraction method |
| CN105347352B (en) * | 2015-12-09 | 2019-03-08 | 李洪岭 | A kind of high-efficiency energy-saving heat reverse-extraction method production boric acid new process |
| CN108017067A (en) * | 2017-12-08 | 2018-05-11 | 中国科学院青海盐湖研究所 | The extraction system and its extracting process of boric acid are extracted from lake bittern water containing magnesium salts |
| CN109126200A (en) * | 2018-08-30 | 2019-01-04 | 山东省医学科学院药物研究所（山东省抗衰老研究中心、山东省新技术制药研究所） | The method of boric acid is extracted from the old halogen of high magnesium and mentions boron extractant |
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|---|---|
| CN101544378B (en) | 2010-12-29 |
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