CN101318675A - Method for removing boron and iron from boron containing magnesium chloride saturated liquid - Google Patents
Method for removing boron and iron from boron containing magnesium chloride saturated liquid Download PDFInfo
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- CN101318675A CN101318675A CNA2008101358526A CN200810135852A CN101318675A CN 101318675 A CN101318675 A CN 101318675A CN A2008101358526 A CNA2008101358526 A CN A2008101358526A CN 200810135852 A CN200810135852 A CN 200810135852A CN 101318675 A CN101318675 A CN 101318675A
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- magnesium chloride
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Abstract
The invention pertains to the technical field of inorganic salt chemical industry, and in particular relates to a method for removing boron and iron from a saturated boron-bearing magnesium chloride solution. The method is a coordinate process integrating acidification and extraction which aims at solving the deficiency of the present process for removing boron and iron from the saturated boron-bearing magnesium chloride solution in salt lakes, and the technological process includes an acidification and boron extraction section, a filtration section, an extraction section and a reverse extraction section. The saturated boron-bearing magnesium chloride solution is taken as the raw material in the method, to which hydrochloric acid or sulfuric acid is added to acidify and precipitate boric acid, the remnant boric acid in the acidizing solution is extracted and removed by a mixed alcohol, the contents of B2O3 and Fe2O3 can be reduced to be less than 25mg/l, and the recovery ratio of boric acid reaches more than 99%; owing to the adoption of the mixed alcohol extraction technology, the method not only solves the problem of great extractant loss in the extraction method effectively, but also removes iron from the saturated magnesium chloride solution, and has the advantages of short technological process, simple operation and high yield.
Description
One, technical field
The invention belongs to the chemical industry of inorganic salt technical field, relate in particular to a kind of from boron containing magnesium chloride saturated liquid the method for removing boron and iron.
Two, technical background
Compose in the salt lake, the Caidamu Basin and have the salt of enriching Mineral resources, main useful element has potassium, sodium, magnesium, boron, lithium etc., wherein boron, magnesium, lithium are enriched in and carry in the potassium post chlorization magnesium saturated solution, can have huge utility value from wherein extracting lithium salts, borate and high-purity magnesium salts.But most of high purity magnesium product salt all requires very low boron and iron content, so exploitation is extracted boric acid and removed the technology of remaining boron and iron from boron containing magnesium chloride saturated liquid, is a key technology of boron in the bittern of the Caidamu Basin, magnesium resource comprehensive utilization.
Boric acid is a kind of important Inorganic Chemicals, is widely used in industrial sectors such as national defence, chemical industry, electronics, medicine, metallurgy, machinery, and purposes is increasingly extensive in modern industry.China's boron resource reserve is not abundant, its total amount only accounts for 12% of world's boron total resources, commercial mining through decades, China has formed suitable scale to the utilization in solid boron rock (boron magnesium ore deposit), and technology is ripe relatively, and the commercial mining of boron in the salt lake brine still is in the starting stage, at present, China's solid boron resource is closely exhausted, but only surplus in the of 300 ten thousand tons of development reserves can not satisfy growing industrial requirement.
Compose the considerable liquid boron resource of memory space in China's Salt Lake on Qinghai-Tibetan Plateau bittern, wherein can be for the salt lake bittern boron resource reserves (B of exploitation
2O
3) above 2,000 ten thousand tons.Extract boric acid one and have 3 kinds of methods from bittern, the main acidization that adopts extracts boric acid at present, and this method is only applicable to contain B
2O
3The bittern of＞20g/l still has 6～7g/lB in the bittern behind the extraction boric acid
2O
3Exist, the thick boric acid rate of recovery is 70～75% after the acidifying, and the rate of recovery is relatively low, and this method is for B
2O
3It is inapplicable that content is lower than the salt lake bittern of 10g/l.Second method is efficient boron resin method, utilizes this resin can be with the boron in the bittern (with B
2O
3Meter) carry to 10mg/l, the boron rate of recovery＞99%, but this method has an obvious shortcoming, namely requires the B in the raw brine
2O
3＜500mg/l, and the salinity of bittern is more low more good, generally is used for seawater and carries boron, is not suitable for to contain B
2O
3Reach the salt lake bittern of 6～10g/l.The third method is extraction, namely adopts the boron in branched alcohol and the bittern to form boron alcohol complex, is dissolved in the organic solvent and finishes extraction process, and this method can be with the boron in the bittern (with B
2O
3Meter) carry to 20mg/l, the boron rate of recovery＞99% is carried boron efficient height, and is applicable to and contains B
2O
3Reach the high salinity salt lake bittern of 6～10g/l, be that a kind of comparatively desirable salt lake bittern is put forward the boron method, have certain water-solublely but the shortcoming of this method maximum is branched-chain alcoho that the extraction process solution loss is big, single extraction solution loss reaches more than 1%, thereby has limited greatly its large-scale application.
Three, summary of the invention
A kind of acidifying that The present invention be directed to the deficiency of boron containing magnesium chloride saturated liquid removing boron and iron technology in the existing salt lake and design, the extraction process integration, the technical scheme that the present invention intends taking is: a kind of from boron containing magnesium chloride saturated liquid the method for removing boron and iron, its technological process is: boron workshop section is carried in acidifying, filter workshop section, extraction workshop section, reextraction workshop section, the processing condition that boron workshop section is carried in acidifying are: add hydrochloric acid or sulfuric acid in boron containing magnesium chloride saturated liquid, adjusting the slip pH value is 1～3, stirring at normal temperature reaction 30～60 minutes, the processing condition of filtering workshop section are: above-mentioned slurry filtration is obtained thick boric acid and acidizing fluid, thick boric acid is made with extra care and is obtained boric acid, acidizing fluid changes subsequent processing over to, the processing condition of extraction workshop section are: add extraction agent and carry out the extraction of 5～10 stage countercurrents in acidizing fluid, it is in a ratio of acidizing fluid: extraction agent=1: 0.5～1.5, mixing time 3～20 minutes, 1～20 minute phase-splitting time, obtain raffinate and saturated organic phase, raffinate is the low iron magnesium chloride saturated liquid of low boron, this saturated solution is used to prepare high-purity magnesium salts, saturated organic phase changes subsequent processing over to, the processing condition of reextraction workshop section are: add entry and carry out the reextraction of 5～8 stage countercurrents in saturated organic phase, it is in a ratio of saturated organic phase: water=1: 0.5～1.5, mixing time 3～20 minutes, 1～20 minute phase-splitting time, obtain strip liquor and regeneration organic phase, boronic acid containing and iron in the strip liquor, the further refining boric acid that obtains, the regeneration organic phase is returned extraction workshop section as extraction agent.Extraction agent is composite extraction agent, its compound method is that secondary octanol and isooctyl alcohol or primary isoamyl alcohol or 2-enanthol contain the branched monobasic alcohol mixture in C5～10 by the composite main chain that obtains of 1: 5～20 mixed, and alcohol mixture obtains composite extraction agent with aviation kerosene or semi-annular jade pendant kerosene by 1: 1 dilution proportion;
The present invention is with boron containing magnesium chloride saturated liquid (B
2O
36～10g/l) is raw material, adds hydrochloric acid or sulfuric acid, and acid precipitation boric acid removes remaining boric acid and iron in the acidifying solution with the mixed alcohol extraction then, can be with B wherein
2O
3And Fe
2O
3Content is to 25mg/l, and the boric acid rate of recovery reaches more than 99%; Owing to adopt the mixed alcohol abstraction technique, not only efficiently solve the big difficult problem of the molten damage of extractant, but also removed the iron in the magnesium chloride saturated liquid; It is short, simple to operate to have technological process, the yield advantages of higher.
Four, description of drawings
Fig. 1 is a process flow sheet of the present invention
Five, embodiment
Embodiment 1
A kind of from boron containing magnesium chloride saturated liquid the method for removing boron and iron, in boron containing magnesium chloride saturated liquid, add sulfuric acid, adjusting the slip pH value is 1, stirring at normal temperature reaction 30 minutes, filter slip and obtain thick boric acid and acidifying solution, thick boric acid is made with extra care and is obtained boric acid, gets acidifying solution (B
2O
37.5g/l, Fe
2O
3130mg/l) 400 milliliters, add 600 milliliters of mixing of extractant, mix to be placed in 1500 milliliters of separatory funnels and shook 20 minutes, leave standstill rear phase-splitting, 1 minute phase-splitting time, carry out the extraction of 10 stage countercurrents, finally obtain saturated organic phase and raffinate, raffinate is the low iron magnesium chloride saturated liquid of low boron, B in the raffinate
2O
3Content is lower than 25mg/l, Fe
2O
322mg/l, the boron rate of recovery＞99%, this saturated solution is for the preparation of high-purity magnesium salts, 400 milliliters of saturated organic phases that obtains enter back extraction, back extraction is in a ratio of 1: 1.5, and strip liquor is fresh water, inserts in 1500 milliliters of separatory funnels to shake 3 minutes, leave standstill rear phase-splitting, 1 minute phase-splitting time, 5 grades of countercurrent reextractions, 600 milliliters of acquisition boracic strip liquors and regeneration organic phase were 400 milliliters after back extraction was finished, strip liquor is the refining boric acid that obtains further, and the regeneration organic phase is returned extraction workshop section as extractant and recycled.Extraction agent is composite extraction agent, and its compound method is that secondary octanol and isooctyl alcohol contain the branched monobasic alcohol mixture in C5～10 by the composite main chain that obtains of 1: 5 mixed, and the monobasic alcohol mixture obtains composite extraction agent with aviation kerosene by 1: 1 dilution proportion;
Embodiment 2
A kind of from boron containing magnesium chloride saturated liquid the method for removing boron and iron, in boron containing magnesium chloride saturated liquid, add sulfuric acid, adjusting the slip pH value is 3, stirring at normal temperature reaction 60 minutes, filter slip and obtain thick boric acid and acidifying solution, thick boric acid is made with extra care and is obtained boric acid, gets acidifying solution (B
2O
37.5g/l, Fe
2O
3130mg/l) 400 milliliters, add 400 milliliters of mixing of extractant, mix to be placed in 1000 milliliters of separatory funnels and shook 3 minutes, leave standstill rear phase-splitting, 20 minutes phase-splitting time, carry out the extraction of 7 stage countercurrents, finally obtain saturated organic phase and raffinate, raffinate is the low iron magnesium chloride saturated liquid of low boron, B in the raffinate
2O
3Content is lower than 20mg/l, Fe
2O
320mg/l, the boron rate of recovery＞99%, this saturated solution is for the preparation of high-purity magnesium salts, 400 milliliters of saturated organic phases that obtains enter back extraction, back extraction is in a ratio of 1: 0.5, and strip liquor is fresh water, inserts in 1000 milliliters of separatory funnels to shake 20 minutes, leave standstill rear phase-splitting, 20 minutes phase-splitting time, 8 grades of countercurrent reextractions, 200 milliliters of acquisition boracic strip liquors and regeneration organic phase were 400 milliliters after back extraction was finished, strip liquor is the refining boric acid that obtains further, and the regeneration organic phase is returned extraction workshop section as extractant and recycled.Extraction agent is composite extraction agent, and its compound method is that secondary octanol and primary isoamyl alcohol contain the branched monobasic alcohol mixture in C5～10 by the composite main chain that obtains of 1: 20 mixed, and the monobasic alcohol mixture obtains composite extraction agent with semi-annular jade pendant kerosene by 1: 1 dilution proportion;
Embodiment 3
A kind of from boron containing magnesium chloride saturated liquid the method for removing boron and iron, in boron containing magnesium chloride saturated liquid, add sulfuric acid, adjusting the slip pH value is 2, stirring at normal temperature reaction 45 minutes, filter slip and obtain thick boric acid and acidifying solution, thick boric acid is made with extra care and is obtained boric acid, gets acidifying solution (B
2O
37.5g/l, Fe
2O
3130mg/l) 400 milliliters, add 400 milliliters of mixing of extractant, mix to be placed in 1000 milliliters of separatory funnels and shook 15 minutes, leave standstill rear phase-splitting, 15 minutes phase-splitting time, carry out the extraction of 8 stage countercurrents, finally obtain saturated organic phase and raffinate, raffinate is the low iron magnesium chloride saturated liquid of low boron, B in the raffinate
2O
3Content is lower than 23mg/l, Fe
2O
324mg/l, the boron rate of recovery＞99%, this saturated solution is for the preparation of high-purity magnesium salts, 200 milliliters of saturated organic phases that obtains enter back extraction, back extraction is in a ratio of 1: 1, and strip liquor is fresh water, inserts in 1000 milliliters of separatory funnels to shake 15 minutes, leave standstill rear phase-splitting, 15 minutes phase-splitting time, 7 grades of countercurrent reextractions, 400 milliliters of acquisition boracic strip liquors and regeneration organic phase were 400 milliliters after back extraction was finished, strip liquor is the refining boric acid that obtains further, and the regeneration organic phase is returned extraction workshop section as extractant and recycled.Extraction agent is composite extraction agent, and its compound method is that secondary octanol and 2-enanthol contain the branched monobasic alcohol mixture in C5～10 by the composite main chain that obtains of 1: 15 mixed, and the monobasic alcohol mixture obtains composite extraction agent with semi-annular jade pendant kerosene by 1: 1 dilution proportion.
Claims (2)
1, a kind of from boron containing magnesium chloride saturated liquid the method for removing boron and iron, it is characterized in that technological process is: boron workshop section is carried in acidifying, filter workshop section, extraction workshop section, reextraction workshop section, the processing condition that boron workshop section is carried in acidifying are: add hydrochloric acid or sulfuric acid in boron containing magnesium chloride saturated liquid, adjusting the slip pH value is 1～3, stirring at normal temperature reaction 30～60 minutes, the processing condition of filtering workshop section are: above-mentioned slurry filtration is obtained thick boric acid and acidizing fluid, thick boric acid is made with extra care and is obtained boric acid, acidizing fluid changes subsequent processing over to, the processing condition of extraction workshop section are: add extraction agent and carry out the extraction of 5～10 stage countercurrents in acidizing fluid, it is in a ratio of acidizing fluid: extraction agent=1: 0.5～1.5, mixing time 3～20 minutes, 1～20 minute phase-splitting time, obtain raffinate and saturated organic phase, raffinate is the low iron magnesium chloride saturated liquid of low boron, this saturated solution is used to prepare high-purity magnesium salts, saturated organic phase changes subsequent processing over to, the processing condition of reextraction workshop section are: add entry and carry out the reextraction of 5～8 stage countercurrents in saturated organic phase, it is in a ratio of saturated organic phase: water=1: 0.5～1.5, mixing time 3～20 minutes, 1～20 minute phase-splitting time, obtain strip liquor and regeneration organic phase, boronic acid containing and iron in the strip liquor, the further refining boric acid that obtains, the regeneration organic phase is returned extraction workshop section as extraction agent.
2, as claimed in claim 1 a kind of from boron containing magnesium chloride saturated liquid the method for removing boron and iron, it is characterized in that extraction agent is composite extraction agent, its compound method is that secondary octanol and isooctyl alcohol or primary isoamyl alcohol or 2-enanthol contain the branched monobasic alcohol mixture in C5～10 by the composite main chain that obtains of 1: 5～20 mixed, and alcohol mixture obtains composite extraction agent with aviation kerosene or semi-annular jade pendant kerosene by 1: 1 dilution proportion.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101358526A CN101318675A (en) | 2008-07-13 | 2008-07-13 | Method for removing boron and iron from boron containing magnesium chloride saturated liquid |
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|---|---|---|---|
| CNA2008101358526A CN101318675A (en) | 2008-07-13 | 2008-07-13 | Method for removing boron and iron from boron containing magnesium chloride saturated liquid |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102344154A (en) * | 2010-08-04 | 2012-02-08 | 张英才 | Method for preparing high-purity magnesium chloride hexahydrate from waste brine |
| CN102452676A (en) * | 2010-10-26 | 2012-05-16 | 华东理工大学 | Removing method of trace impurity in magnesium chloride |
| 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 |
| CN102618932A (en) * | 2012-03-31 | 2012-08-01 | 合肥工业大学 | Method for preparing basic ammonium aluminum carbonate hydroxide whisker and aluminum oxide whisker co-production liquid sodium silicate from bentonite |
| CN105198054A (en) * | 2014-06-10 | 2015-12-30 | 中国科学院过程工程研究所 | Method for removing boron in water body |
| CN105293652A (en) * | 2014-06-10 | 2016-02-03 | 中国科学院过程工程研究所 | Method for removing boron from water by using magnesite |
| CN106219564A (en) * | 2016-08-17 | 2016-12-14 | 青海柴达木兴华锂盐有限公司 | Box extraction tank is the application of boron in extraction salt lake bittern |
| CN106587090A (en) * | 2016-12-23 | 2017-04-26 | 江西合纵锂业科技有限公司 | Method for synthesizing disodium octaborate tetrahydrate by utilizing liquid boron ore |
| CN107459163A (en) * | 2017-07-28 | 2017-12-12 | 江苏昌吉利新能源科技有限公司 | A kind of extraction boron removal method of the bittern containing lithium |
-
2008
- 2008-07-13 CN CNA2008101358526A patent/CN101318675A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102344154A (en) * | 2010-08-04 | 2012-02-08 | 张英才 | Method for preparing high-purity magnesium chloride hexahydrate from waste brine |
| CN102452676B (en) * | 2010-10-26 | 2014-04-23 | 华东理工大学 | Removing method of trace impurity in magnesium chloride |
| CN102452676A (en) * | 2010-10-26 | 2012-05-16 | 华东理工大学 | Removing method of trace impurity in magnesium chloride |
| CN102618932B (en) * | 2012-03-31 | 2015-03-25 | 合肥工业大学 | Method for preparing basic ammonium aluminum carbonate hydroxide whisker and aluminum oxide whisker co-production liquid sodium silicate from bentonite |
| CN102618932A (en) * | 2012-03-31 | 2012-08-01 | 合肥工业大学 | Method for preparing basic ammonium aluminum carbonate hydroxide whisker and aluminum oxide whisker co-production liquid sodium silicate from bentonite |
| 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 |
| 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 |
| CN105198054A (en) * | 2014-06-10 | 2015-12-30 | 中国科学院过程工程研究所 | Method for removing boron in water body |
| CN105293652A (en) * | 2014-06-10 | 2016-02-03 | 中国科学院过程工程研究所 | Method for removing boron from water by using magnesite |
| CN105293652B (en) * | 2014-06-10 | 2018-06-22 | 中国科学院过程工程研究所 | It is a kind of to carry out method of the water body except boron using magnesite |
| CN106219564A (en) * | 2016-08-17 | 2016-12-14 | 青海柴达木兴华锂盐有限公司 | Box extraction tank is the application of boron in extraction salt lake bittern |
| CN106587090A (en) * | 2016-12-23 | 2017-04-26 | 江西合纵锂业科技有限公司 | Method for synthesizing disodium octaborate tetrahydrate by utilizing liquid boron ore |
| CN106587090B (en) * | 2016-12-23 | 2018-11-13 | 江西合纵锂业科技有限公司 | A method of synthesizing four water eight borate two sodium using liquid boron rock |
| CN107459163A (en) * | 2017-07-28 | 2017-12-12 | 江苏昌吉利新能源科技有限公司 | A kind of extraction boron removal method of the bittern containing lithium |
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