CN105314665B - One kind compounding ferric sulfate extractant - Google Patents
One kind compounding ferric sulfate extractant Download PDFInfo
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- CN105314665B CN105314665B CN201410338657.9A CN201410338657A CN105314665B CN 105314665 B CN105314665 B CN 105314665B CN 201410338657 A CN201410338657 A CN 201410338657A CN 105314665 B CN105314665 B CN 105314665B
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- extractant
- extraction
- ferric sulfate
- ethylhexyl
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Abstract
Ferric sulfate extractant is compounded the present invention relates to one kind, the extractant main component includes the one or more in the ethylhexyl of 2 ethylhexyl phosphonic acid mono 2, two (2 ethylhexyl) phosphoric acid, trioctylamine and TBP, and diluent is kerosene.The present invention efficiently solves the technical barrier that aluminum sulfate separates sulfuric acid iron tramp, and its technical advantage includes：Modifying agent TBP is used in extraction system, emulsification and the extraction split-phase of extractant can be effectively solved the problems, such as, shorten extraction time, it is cost-effective；Extraction only needs to coagulation with back extraction and can reach>97% extraction yield and back extraction ratio, product aluminum sulfate reaches the standard of the raw material of metallurgical-grade aluminum oxide；Extractant is recycled；Flow is simple, and process environmental protection, good separating effect, production efficiency is high, with cost advantage, is easy to industrialization.
Description
【Technical field】
It is a kind of compounding ferric sulfate extractant specifically the present invention relates to ferric sulfate abstraction technique field.
【Background technology】
Aluminum sulfate is a kind of important industrial chemicals, in terms of being decolourized available for water process, papermaking, manufacture alum, oil.
The height of iron content, directly affects product quality in industrial aluminum sulphate.With the development of the industries such as papermaking, food, catalysis, low iron
The demand of aluminum sulfate or non-iron aluminium sulfate is increasing, therefore studies from Aluminum Sulfate Solution except iron is significant.
In recent years, the research except iron from aluminum sulfate is more, and main method has recrystallization method, the precipitation method, alcohol to wash method and molten
Agent extraction, such as United States Patent (USP) US4039615, China Patent Publication No. CN1559906A, China Patent Publication No.
Side disclosed in CN101659438A, China Patent Publication No. CN102660679A, China Patent Publication No. CN86100720A etc.
Method.First three methods exist to some extent complex operation, be difficult to filter, the low shortcoming for the treatment of effeciency.And solvent extraction has
The advantages of good separating effect, production efficiency are high, secondary pollution is small.
【The content of the invention】
Ferric sulfate extractant is compounded it is an object of the invention to overcome the deficiencies of the prior art and provide one kind.
The purpose of the present invention is achieved through the following technical solutions：
One kind compounding ferric sulfate extractant, its raw material constitutes percent by volume and is：
Described kerosene is sulfonated kerosene or aviation kerosine.
The volume fraction of described di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester is 15~20%；
The volume fraction of described di-(2-ethylhexyl)phosphoric acid is 15~20%；
The volume fraction of described trioctylamine is 35~40%；
Described tributyl phosphate TBP volume fraction is 4~6% or 7~8%；
Above-mentioned efficient ferric sulfate compounding extractant is added in aluminum sulfate material solution and carries out one or more levels extraction, separation
The extract gone out is stripped with dilute sulfuric acid, and product aluminum sulfate can reach the standard of the raw material of metallurgical-grade aluminum oxide.
The inventive method extractant when being extracted is recommended as compared with material：O/A=0.5/1~1.5/1；Back extraction
When organic phase and back washing agent be in a ratio of O/A=0.5/1~1.5/1.The temperature of system is recommended as 10 when extraction is with back extraction operation
~50 DEG C.
The concrete technology of the present invention is industrial high-iron aluminum sulfate (iron content Al2O3/Fe2O3=10~50) plus appropriate water-soluble
Solve as the aluminum sulfate solution of sulfur acid iron, the extractant compounded with the present invention is extracted, the standing point after fully reaction stirring
Layer, aqueous phase can obtain metallurgical grade high-purity sulphuric acid aluminium by crystallization, and organic phase can be continued cycling through after being stripped through dilute sulfuric acid and used.In detail
The visible Fig. 1 of technique.
The structural formula of di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester is as follows：
The structural formula of di-(2-ethylhexyl)phosphoric acid is as follows：
The structural formula of trioctylamine is as follows：
Tributyl phosphate TBP structural formulas are as follows：
Compared with prior art, the positive effect of the present invention is：
(1) modifying agent TBP is used in extraction system of the invention, the emulsification and extraction split-phase that can effectively solve extractant are asked
Topic, shortens extraction time, cost-effective；
(2) extraction process of the invention only needs to coagulation and can reach with being stripped>97% extraction yield with
Back extraction ratio, product aluminum sulfate reaches the standard of the raw material as metallurgical-grade aluminum oxide, does not substantially introduce any additional in product
Other metal cations and other anion；
(3) whole technological process does not produce pollutant, agents useful for same all reusable edibles substantially.
【Brief description of the drawings】
The process chart of Fig. 1 present invention.
【Embodiment】
A kind of embodiment for compounding ferric sulfate extractant of the present invention presented below.
Embodiment 1
150mL aluminum sulfate solutions, wherein Al are added in volume is 500mL bulb shape separatory funnel2O3108.47g/L contain
Amount, Fe2O3Content 2.71g/L, solution ph is 1.83, adds 150mL compositions and is：2- ethylhexyl phosphonic acid mono 2- ethylhexyls
Ester 20%, di-(2-ethylhexyl)phosphoric acid 10%, trioctylamine 34%, TBP6%, the compounding extractant of kerosene 30% is in room temperature bar
15~20min is sufficiently mixed under part, then 10~25min of stratification.The rate of recovery of aluminium is 97.11% in aqueous phase, and iron is gone
Except rate is 97.58%.Organic phase is stripped through 1mol/L dilute sulfuric acids 1: 1, and back extraction ratio is more than 99%.
Embodiment 2
150mL aluminum sulfate solutions, wherein Al are added in volume is 500mL bulb shape separatory funnel2O3108.47g/L contain
Amount, Fe2O3Content 2.71g/L, solution ph is 1.83, adds 150mL compositions and is：2- ethylhexyl phosphonic acid mono 2- ethylhexyls
Ester 15%, di-(2-ethylhexyl)phosphoric acid 20%, trioctylamine 45%, TBP4%, the compounding extractant of kerosene 16% is in room temperature bar
15~20min is sufficiently mixed under part, then 10~25min of stratification.The rate of recovery of aluminium is 96.11% in aqueous phase, and iron is gone
Except rate is 98.58%.Organic phase is stripped through 1mol/L dilute sulfuric acids 1: 1, and back extraction ratio is more than 99%.
Embodiment 3
150mL aluminum sulfate solutions, wherein Al are added in volume is 500mL bulb shape separatory funnel2O3112.73g/L contain
Amount, Fe2O3Content 2.98g/L, solution ph is 1.87, adds 180mL compositions and is：2- ethylhexyl phosphonic acid mono 2- ethylhexyls
Ester 30%, di-(2-ethylhexyl)phosphoric acid 15%, trioctylamine 20%, TBP2%, the compounding extractant of kerosene 33% is in room temperature bar
20-25min is sufficiently mixed under part, then 10~25min of stratification.The rate of recovery of aluminium is 97.29%, the removal of iron in aqueous phase
Rate is 97.79%.Organic phase is stripped through 1mol/L dilute sulfuric acids 1: 1, and back extraction ratio is more than 99%.
Embodiment 4
150mL aluminum sulfate solutions, wherein Al are added in volume is 500mL bulb shape separatory funnel2O3112.73g/L contain
Amount, Fe2O3Content 2.98g/L, solution ph is 1.87, adds 180mL compositions and is：2- ethylhexyl phosphonic acid mono 2- ethylhexyls
Ester 20%, di-(2-ethylhexyl)phosphoric acid 20%, trioctylamine 40%, TBP2%, the compounding extractant of kerosene 18% is in room temperature bar
20-25min is sufficiently mixed under part, then 10~25min of stratification.The rate of recovery of aluminium is 98.39%, the removal of iron in aqueous phase
Rate is 98.69%.Organic phase is stripped through 1mol/L dilute sulfuric acids 1: 1, and back extraction ratio is more than 99%.
Comparative example 1
150mL aluminum sulfate solutions are separately added into 2 volumes is 500mL bulb shape separatory funnels, wherein
Al2O3105.64g/L content, Fe2O3Content 2.82g/L, solution ph is 1.85, adds 150mL compositions and is：(1) 2- ethyl hexyls
Base phosphonic acids single 2-ethyl hexyl ester 20%, TBP5%, the compounding extractant of kerosene 75%；(2) trioctylamine 30%, TBP5%, coal
The compounding extractant of oil 65%, in being sufficiently mixed 15-20min under room temperature condition, then stratification 10-25min, the removal of iron
Rate is (1) 68.47%；(2) 66.51%.
Comparative example 2
150mL aluminum sulfate solutions are separately added into 2 volumes is 500mL bulb shape separatory funnels, wherein
Al2O3114.67g/L content, Fe2O3Content 2.50g/L, solution ph is 1.81, adds 150mL compositions and is：(1) 2- ethyl hexyls
Base phosphonic acids single 2-ethyl hexyl ester 20%, the compounding extractant of kerosene 80%；(2) trioctylamine 30%, the compounding extraction of kerosene 70%
Agent is taken, in being sufficiently mixed 15-20min under room temperature condition, then stratification is more than 30min, and the clearance of iron is (1)
69.91%；(2) 65.47%.(1) is tested due to the emulsification of phosphate, occurs white vaporific phenomenon in its aqueous solution,
Layering is slow.
By comparative example as can be seen that the present invention efficiently solves the technical barrier that aluminum sulfate separates sulfuric acid iron tramp, its
Technical advantage includes：Modifying agent TBP is used in extraction system, emulsification and the extraction split-phase of extractant, contracting can be effectively solved the problems, such as
Short extraction time, it is cost-effective；Extraction only needs to coagulation with back extraction and can reach>97% extraction yield and back extraction ratio,
Product aluminum sulfate reaches the standard of the raw material of metallurgical-grade aluminum oxide；Extractant is recycled；Flow is simple, process environmental protection, separation
Effect is good, and production efficiency is high, with cost advantage, is easy to industrialization.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
Member, without departing from the inventive concept of the premise, can also make some improvements and modifications, these improvements and modifications also should be regarded as
In protection scope of the present invention.
Claims (3)
1. one kind compounding ferric sulfate extractant, it is characterised in that its raw material constitutes percent by volume and is：
Above-mentioned efficient ferric sulfate compounding extractant is added in aluminum sulfate material solution and carries out one or more levels extraction, is isolated
Extract is stripped with dilute sulfuric acid, and product aluminum sulfate reaches the standard of the raw material of metallurgical-grade aluminum oxide.
2. a kind of compounding ferric sulfate extractant as claimed in claim 1, it is characterised in that extractant and thing when being extracted
That expects is in a ratio of：O/A=0.5/1~1.5/1；Organic phase and back washing agent is in a ratio of O/A=0.5/1~1.5/1 during back extraction；Extraction
The temperature of system during with back extraction operation is taken to be recommended as 10~50 DEG C.
3. compounding ferric sulfate extractant as claimed in claim 1 a kind of, it is characterised in that described kerosene be sulfonated kerosene or
Aviation kerosine.
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| CN201410338657.9A CN105314665B (en) | 2014-07-16 | 2014-07-16 | One kind compounding ferric sulfate extractant |
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| CN201410338657.9A CN105314665B (en) | 2014-07-16 | 2014-07-16 | One kind compounding ferric sulfate extractant |
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| CN105314665A CN105314665A (en) | 2016-02-10 |
| CN105314665B true CN105314665B (en) | 2017-10-31 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106745142B (en) * | 2017-01-19 | 2018-01-26 | 济南大学 | A kind of extracting process for preparing high-purity aluminium chloride |
| CN106892479B (en) * | 2017-03-13 | 2020-07-03 | 东北大学 | Method for recovering oxalic acid and hydrochloric acid from rare earth oxalic acid precipitation wastewater |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85100736A (en) * | 1985-04-01 | 1986-07-30 | 中国科学院化工冶金研究所 | In sulfate liquor, extract deironing |
| CN1031859A (en) * | 1987-07-02 | 1989-03-22 | 中国科学院化工冶金研究所 | Phase transition back extraction in acid phosphorus (phosphine) the acid esters collection iron |
-
2014
- 2014-07-16 CN CN201410338657.9A patent/CN105314665B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85100736A (en) * | 1985-04-01 | 1986-07-30 | 中国科学院化工冶金研究所 | In sulfate liquor, extract deironing |
| CN1031859A (en) * | 1987-07-02 | 1989-03-22 | 中国科学院化工冶金研究所 | Phase transition back extraction in acid phosphorus (phosphine) the acid esters collection iron |
Non-Patent Citations (3)
| Title |
|---|
| 溶剂萃取法从含铁硫酸铝溶液中除铁的工艺研究;黄伦光;《湿法冶金》;19980630;第2、5.2、5.3节，表3、4，图7 * |
| 溶剂萃取法从硫酸介质中除铁;李雁南;《湿法冶金》;19960331;全文 * |
| 用叔胺N235从硫酸铝溶液中萃取除铁;吴成友;《湿法冶金》;20120630;全文 * |
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