CN104760938B - A kind of method of iron ion in removal concentrated sulfuric acid - Google Patents
A kind of method of iron ion in removal concentrated sulfuric acid Download PDFInfo
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- CN104760938B CN104760938B CN201510132190.7A CN201510132190A CN104760938B CN 104760938 B CN104760938 B CN 104760938B CN 201510132190 A CN201510132190 A CN 201510132190A CN 104760938 B CN104760938 B CN 104760938B
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- sulfuric acid
- concentrated sulfuric
- iron ion
- chlorination
- iron
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Abstract
The present invention relates to a kind of reaction, extraction method for removing iron ion in the concentrated sulfuric acid, this method is by the way that a kind of ionic liquid (the methylimidazole purity of 1 ethyl of chlorination 3 is 99%) is added into the concentrated sulfuric acid containing iron ion with concentrated hydrochloric acid, 50 DEG C of oil baths, magnetic agitation, 1.5 hours are reacted with iron ion, then petroleum ether is added to be extracted, organic phase is stripped using sodium hydroxide simultaneously, obtain iron hydroxide, the methylimidazole of 1 ethyl of chlorination 3 and extractant, ionic liquid and extractant are recycled, and the clearance of iron ion is up to 85% in the concentrated sulfuric acid.The present invention has：The advantages of impurity that equipment investment is small, process conditions are gentle, easy to operate, cost is low, bring into is few.
Description
Technical field
The present invention relates to a kind of reaction, extraction technology, more particularly, to anti-used in iron ion in one kind removal concentrated sulfuric acid
Answer abstraction technique.
Background technology
At present, in chemical production processing technology, the concentrated sulfuric acid is a kind of important raw material, as battery liquid, and dense
Sulfuric acid, which can be produced or joined in production or transportation, a small amount of iron ion, and influence product is used and class.With modern production work
The requirement more and more higher of skill or downstream production technology, producer requires have a kind of product to be gone on the premise of its technique is basically unchanged
Iron ions content.The method of iron ions is gone mainly to have cationic ion-exchange resin, peroxide passivation, the way of distillation at present.But these
Method cost is big (such as due to the influence of impurity in acid solution, resin life is shorter, and the replacing frequency is sometimes higher, and cost is big), double
The bad control feeding quantity of oxygen water law, way of distillation technique is cumbersome, and cost of investment is too high.And iron ion can be generated with ionic liquid and is complexed
Thing, taking ionic liquid reaction, extraction method to remove iron ion in the concentrated sulfuric acid has：Equipment investment is small, process conditions are gentle, easily
Operation, the advantages of cost is low, the impurity brought into is few.The iron ion in the concentrated sulfuric acid is separated using reaction, extraction method, can not only be changed
Enter deferrization process, and ferric oxide red colorant can also be obtained using accessory substance iron hydroxide, for the sustainable of sulfuric acid industry
Development has important practical significance.
The content of the invention
The weak point existed for current concentrated sulfuric acid deferrization process, the present invention provides a kind of reaction, extraction technology and removes iron
The method of ion, can effectively simplify iron ion removing program in the concentrated sulfuric acid, further improve the performance of the concentrated sulfuric acid.
The technical process of the inventive method is as follows.
Using the concentrated sulfuric acid of copper smelting by pyrometallurgy by-product as raw material, by mass percentage, iron ion content is 80000 to ten thousand/10000ths
/ ten.Iron is removed using reaction, extraction, concentrated hydrochloric acid, chlorination 1- ethyl-3-methylimidazoles ([EMIM] are sequentially added to the concentrated sulfuric acid
Cl complex reaction) is carried out, concentrated hydrochloric acid addition is 0.8-1.0 milliliters, and chlorination 1- ethyl-3-methylimidazoles addition is 0.4-
0.5 gram, 50 DEG C of oil baths, magnetic agitation after reacting 1.5 hours, is extracted with petroleum ether, fully vibration, static, and layering is obtained
It is mutually concentrated sulfuric acid solution to non-organic, obtains complex compound and extractant that organic phase is iron content, then adding mass concentration is
10% sodium hydroxide solution is stripped to organic phase, and the addition for controlling sodium hydroxide solution is the 7%- of organic phase volume
10%, regulation pH value is 9, fully vibration, is stood, and layering obtains iron hydroxide, chlorination 1- ethyl-3-methylimidazoles and extraction
Agent, ion liquid abstraction agent is recycled.Using the concentration of atomic absorption spectrophotometric determination iron ion, iron ion in the concentrated sulfuric acid
Reachable clearance is 85%.
The principle reaction of the present invention is as follows：
Occur complex reaction in concentrated sulfuric acid first, then extracted using petroleum ether, organic phase is stripped,
Its reaction equation is：
[EMIM]Cl+3HCl+Fe3+→[EMIM]FeCl4+3H-
[EMIM]FeCl4+3NaOH→[EMIM]Cl+3NaCl+Fe(OH)3↓
It is of the invention compared with other related removal technologies, most outstanding feature is：Technological process is simple, and equipment investment is small,
Reaction condition is easily controllable, and process conditions require low, and the impurity brought into is few, and the obtained concentrated sulfuric acid disclosure satisfy that as accumulator green
To the requirement of the concentrated sulfuric acid in production.
Brief description of the drawings
Fig. 1 is the process chart that iron ion in the concentrated sulfuric acid is removed in the present invention.
Embodiment
Pipette 100 milliliters of iron ion contents be 0.0009 (mass percent) the concentrated sulfuric acid in 400 milliliters of beakers, add
0.8 milliliter of concentrated hydrochloric acid, adds 0.45 gram of chlorination 1- ethyl-3-methylimidazoles, puts in 50 DEG C of oil baths, magnetic agitation, and reaction 1.5 is small
Shi Hou, is extracted with 40 milliliters of petroleum ethers, fully vibration, static, layering, and it is mutually concentrated sulfuric acid solution to obtain non-organic, is obtained
Organic phase is the complex compound and extractant of iron content, and then 3.5 milliliters of mass concentrations of addition are 10% sodium hydroxide solution to organic
Mutually it is stripped, fully vibration, is stood, layering obtains iron hydroxide, chlorination 1- ethyl-3-methylimidazoles and extractant, dense
The clearance of iron ion is 85.2% in sulfuric acid.
Claims (1)
1. going the method for iron ions in a kind of concentrated sulfuric acid, its feature adds a certain amount of dense salt using the iron content concentrated sulfuric acid as raw material
Acid, chlorination 1- ethyl-3-methylimidazoles carry out complex reaction, and in 50 DEG C of oil baths, magnetic agitation 1.5 hours is carried out with petroleum ether
Extraction, fully vibration, static, layering then add a certain amount of mass concentration and organic phase are carried out for 10% sodium hydroxide solution
Back extraction, fully vibration, stand, and layering obtains iron hydroxide, chlorination 1- ethyl-3-methylimidazoles and petroleum ether, chlorination 1- second
Base -3- methylimidazoles and petroleum ether are recycled, and iron ion removing rate is up to 85%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510132190.7A CN104760938B (en) | 2015-03-18 | 2015-03-18 | A kind of method of iron ion in removal concentrated sulfuric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510132190.7A CN104760938B (en) | 2015-03-18 | 2015-03-18 | A kind of method of iron ion in removal concentrated sulfuric acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104760938A CN104760938A (en) | 2015-07-08 |
| CN104760938B true CN104760938B (en) | 2017-10-13 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510132190.7A Expired - Fee Related CN104760938B (en) | 2015-03-18 | 2015-03-18 | A kind of method of iron ion in removal concentrated sulfuric acid |
Country Status (1)
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105624399B (en) * | 2016-02-04 | 2017-12-05 | 山西大学 | A kind of method that iron removaling is stripped from rich iron ion liquid |
| CN108179273A (en) * | 2018-01-19 | 2018-06-19 | 重庆康普化学工业股份有限公司 | A kind of method using solvent-extracted back extraction iron |
| CN110092358A (en) * | 2019-05-24 | 2019-08-06 | 华东理工大学 | A kind of processing method of waste sulfuric acid from alkylation |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2968877B2 (en) * | 1991-11-08 | 1999-11-02 | 日鉄鉱業株式会社 | Method for recovering sulfuric acid from waste sulfuric acid containing metal sulfate |
| CN1936035A (en) * | 2006-09-29 | 2007-03-28 | 金川集团有限公司 | P204 deferrizing regeneration method |
| CN101514165B (en) * | 2009-03-24 | 2012-09-05 | 中国科学院长春应用化学研究所 | Method for preparing liquid containing metallic ions by employing extraction reaction |
| CN103160689B (en) * | 2013-02-26 | 2014-11-05 | 中南大学 | Method of iron extraction and removal with solvent extraction agent |
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2015
- 2015-03-18 CN CN201510132190.7A patent/CN104760938B/en not_active Expired - Fee Related
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| CN104760938A (en) | 2015-07-08 |
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Granted publication date: 20171013 Termination date: 20180318 |