CN106745142B - A kind of extracting process for preparing high-purity aluminium chloride - Google Patents
A kind of extracting process for preparing high-purity aluminium chloride Download PDFInfo
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- CN106745142B CN106745142B CN201710038434.4A CN201710038434A CN106745142B CN 106745142 B CN106745142 B CN 106745142B CN 201710038434 A CN201710038434 A CN 201710038434A CN 106745142 B CN106745142 B CN 106745142B
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- extraction
- organic phase
- iron
- aluminium chloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/56—Chlorides
- C01F7/62—Purification
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
Abstract
The invention discloses a kind of extraction new method for preparing high-purity aluminium chloride.This method is to utilize extractant N, N, N ' N ' four octyl group 3 oxygen glutaramide extract iron tramp in liquor alumini chloridi, effect of extracting is good.It can be used for the iron and trace iron tramp for extracting the high content in liquor alumini chloridi, it is complete close to extraction.And to the Ca in liquor alumini chloridi2+、Zn2+Effect of extracting is good.Back extraction recycling is carried out to the organic phase after extraction, the recycling of extractant can be achieved.
Description
Technical field
The present invention relates to a kind of extracting process for preparing high-purity aluminium chloride, is studied specifically for purification by liquid extraction, belongs to extraction
Method of purification research field.
Background technology
Purified with the requirement more and more higher to raw material aluminium chloride purity, therefore by existing raw material of industry aluminium chloride
It is particularly important.And iron tramp is common in aluminium chloride and is not easy the impurity removed.Extraction is isolating and purifying industry with weight
Act on, people have carried out substantial amounts of research to abstraction purification, but in face of the removal of trace iron tramp in aluminium chloride, do not facilitate
Effective extracting process.The method of the abstraction purification has very high reality to the abstraction purification of trace iron tramp in industrial chlorinations aluminium
With value and significance, to Ca in liquor alumini chloridi2+、Zn2+Removal also there is important application.
The method of research aluminium chloride purifying mainly has resin anion (R.A.) absorption method, anhydrous Aluminum chloride sublimed method, solution to tie again
Crystallization etc..But these methods are usually complex operation, equipment requirement is high, de-ferrous effect is bad, are extremely difficult to high-purity requirement.
To improve the purity of aluminium chloride, the iron tramp content in aluminium chloride is reduced, or even iron is approached and eliminated, many work
Person has carried out numerous studies.Cui Li etc. are using the iron in Aliquat336 extractions Coal Solid Wastes containing aluminium, six water chlorine after extraction
Change iron content in aluminium and be less than 0.005%；Wei Cundi etc. is using phosphoric acid, the extractant such as acetamide, impurity in the crystal aluminum chloride of preparation
The mass fraction of iron chloride is 0.2-0.3%；Wang XingYao etc. use N235Extract 15gdm-3 Fe3+, 32 gdm-3
Al3+, 40 gdm-3 Ca2+Iron in solution, wherein concentration of hydrochloric acid are 3 moldm-3, ferric ion in solution after extraction
Content be 0.0165 gdm-3.The problems such as above-mentioned extraction system has easily emulsification, extractant is lost in, does not reach high-purity chlorination
Requirement of the aluminium production technology to iron content.
The content of the invention
In view of the above-mentioned problems of the prior art, the present invention provides a kind of extracting process for preparing high-purity aluminium chloride, with
Solve the problems, such as that in the prior art efficiency is low during to iron content liquor alumini chloridi progress iron removaling, cost is high.
To achieve these goals, the invention provides a kind of extracting process for preparing high-purity aluminium chloride, including following step
Suddenly：
（1）By sample deionized water dissolving to be extracted, Al3+Concentration is about 1-3 moldm-3, with analysis pure hydrochloric acid
The concentration of hydrochloric acid for adjusting solution is about 0.01-4 moldm-3；
（2）Preparing includes the extraction organic phase of extractant and diluent, mole of extractant in described extraction organic phase
Concentration is 0.1-0.6 moldm-3, wherein extractant is N, N, N ' and the N octyl group -3- oxygen glutaramides of '-four, diluent is selected from ring
Hexane and n-dodecane；
（3）By step（1）Obtained solution and step（2）Obtained extraction is organic to be mixed to be extracted, and reaches extraction
Make even and organic phase and aqueous phase are separated after weighing, complete single extraction process, the aqueous phase is the liquor alumini chloridi after extraction；
（4）By the aqueous phase continuation after separation and step（2）Obtained extraction is organic to be mixed to be extracted, and reaches extraction
Organic phase and aqueous phase are separated after balance, is so continued after repeating to extract, gained aqueous phase is that the aluminium chloride after multiple continuous extraction is molten
Liquid；
（5）By step（3）And step（4）Extraction after organic phase mixed with aqueous slkali, and with pickling, be stripped
To reclaim organic phase.
In the present invention, step（1）For the preparation of original aqueous phase, by the aluminium chloride sample deionized water dissolving of iron content,
Or a certain amount of iron is added to prepare the liquor alumini chloridi of high content iron impurity.With the pH value of hydrochloric acid regulation liquor alumini chloridi, salt
The preferred concentrated hydrochloric acid of acid.
In the present invention, step（2）The step of to prepare organic phase.The molar concentration of the extractant is 0.1-0.6
mol·dm-3.The extraction organic phase can include extractant and hexamethylene.The extraction organic phase can include extractant and positive ten
Dioxane.Extractant is N, N, N ' the N octyl group -3- oxygen glutaramides of '-four.The method of configuration is not particularly limited.
In the present invention, step（3）For extraction step.Wherein, the volume ratio of the extraction organic phase and aqueous phase can be
1:1, can be 1:2.
In the present invention, in step（3）In, extraction temperature is 20-30 DEG C, and extraction time can be 0.5-2.0 hours.It is excellent
It can be 25 DEG C to select extraction temperature, and extraction time can be 0.5 hour.
In the present invention, step（3）In, the organic phase after extraction and aqueous phase are mixed in extraction equipment, are transferred to point
After being stood in liquid device, organic phase and aqueous phase are divided into two layers up and down.Lower floor's aqueous phase is released and collected, it is molten for the aluminium chloride after extraction
Liquid.
In the present invention, step（4）For multiple continuous extraction, obtained aqueous phase is that the aluminium chloride after multiple continuous extraction is molten
Liquid.
In the present invention, step（5）For strip stage.By step（3）And step（4）Organic phase and carbon after middle extraction
Acid sodium solution mixes, and is stripped to reclaim organic phase.The concentration of sodium carbonate liquor can be 0.1-1 moldm-3.Hydrochloric acid
The concentration of solution can be 1-5 moldm-3。
In the present invention, step（5）It can be carried out in separatory funnel.By the organic phase elder generation after extraction and sodium carbonate liquor
Mixing, then stir 0.3-3 hours.After stratification, organic phase and aqueous phase are separated.Isolated organic phase is molten with hydrochloric acid again
Liquid mixes, and then stirs 0.3-1 hours.After stratification, organic phase and aqueous phase are separated.Isolated organic phase can conduct
New organic phase recycling.
Iron removaling processing is carried out to the liquor alumini chloridi of iron content using the method for the present invention, reduces the use of extractant, has
Iron tramp in effect extraction liquor alumini chloridi.
Beneficial effect
The present invention utilize N, N, N ' the N octyl group of '-four -3- oxygen glutaramides as extractant utilize extraction extract aluminium chloride
Iron tramp in solution, extractant molecules amount is big, not soluble in water, is not lost in；The iron content in solution after extraction is less than detection
The test limit of instrument, the Monitoring lower-cut of inductively coupled plasma spectrophotometer iron content is 4.6 × 10-7g·dm-3.Extraction effect
Fruit is significantly better than current report.
Embodiment
The present invention is further described with reference to embodiment, but the present invention is not therefore subject to any restriction.
Embodiment 1
It is 2.0 moldm to prepare chlorination aluminium content-3, iron tramp content is 0.17gdm-3, concentration of hydrochloric acid 0.01
mol·dm-3Liquor alumini chloridi as aqueous phase.Prepare 0.2 moldm-3N, N, N ' the N octyl group -3- oxygen glutaramides of '-four
Hexamethylene organic phase.It is standby.
Above-mentioned extraction organic phase and aqueous phase are pressed 1 respectively:1 volume ratio mixing, it is 25 DEG C to control extraction temperature, is being extracted
Stirred 0.5 hour in groove.By centrifugation, two phases were separated, and water intaking mutually determines its iron-holder, calculates the extraction yield of corresponding system.From
When the heart separates, the rotating speed of centrifuge is 5000 revs/min.
Specific process parameter and product property are shown in Table 1.
Embodiment 2
It is 2.0 moldm to prepare chlorination aluminium content-3, iron tramp content is 0.17gdm-3, concentration of hydrochloric acid 0.39
mol·dm-3Liquor alumini chloridi as aqueous phase.Prepare 0.2 moldm-3N, N, N ' the N octyl group -3- oxygen glutaramides of '-four
Hexamethylene organic phase.It is standby.
Above-mentioned extraction organic phase and aqueous phase are pressed 1 respectively:1 volume ratio mixing, it is 25 DEG C to control extraction temperature, is being extracted
Stirred 0.5 hour in groove.By centrifugation, two phases were separated, and water intaking mutually determines its iron-holder, calculates the extraction yield of corresponding system.From
When the heart separates, the rotating speed of centrifuge is 5000 revs/min.
Specific process parameter and product property are shown in Table 1.
Embodiment 3
It is 2.0 moldm to prepare chlorination aluminium content-3, iron tramp content is 0.17gdm-3, concentration of hydrochloric acid 1.18
mol·dm-3Liquor alumini chloridi as aqueous phase.Prepare 0.2 moldm-3N, N, N ' the N octyl group -3- oxygen glutaramides of '-four
Hexamethylene organic phase.It is standby.
Above-mentioned extraction organic phase and aqueous phase are pressed 1 respectively:1 volume ratio mixing, it is 25 DEG C to control extraction temperature, is being extracted
Stirred 0.5 hour in groove.By centrifugation, two phases were separated, and water intaking mutually determines its iron-holder, calculates the extraction yield of corresponding system.From
When the heart separates, the rotating speed of centrifuge is 5000 revs/min.
Specific process parameter and product property are shown in Table 1.
Embodiment 4
It is 2.0 moldm to prepare chlorination aluminium content-3, iron tramp content is 0.17gdm-3, concentration of hydrochloric acid 3.15
mol·dm-3Liquor alumini chloridi as aqueous phase.Prepare 0.2 moldm-3N, N, N ' the N octyl group -3- oxygen glutaramides of '-four
Hexamethylene organic phase.It is standby.
Above-mentioned extraction organic phase and aqueous phase are pressed 1 respectively:1 volume ratio mixing, it is 25 DEG C to control extraction temperature, is being extracted
Stirred 0.5 hour in groove.By centrifugation, two phases were separated, and water intaking mutually determines its iron-holder, calculates the extraction yield of corresponding system.From
When the heart separates, the rotating speed of centrifuge is 5000 revs/min.
Specific process parameter and product property are shown in Table 1.
Embodiment 5
It is 2.0 moldm to prepare chlorination aluminium content-3, iron tramp content is 0.17gdm-3, concentration of hydrochloric acid 1.18
mol·dm-3Liquor alumini chloridi as aqueous phase.Prepare 0.1 moldm-3N, N, N ' the N octyl group -3- oxygen glutaramides of '-four
Hexamethylene organic phase.It is standby.
Above-mentioned extraction organic phase and aqueous phase are pressed 1 respectively:1 volume ratio mixing, it is 25 DEG C to control extraction temperature, is being extracted
Stirred 0.5 hour in groove.By centrifugation, two phases were separated, and water intaking mutually determines its iron-holder, calculates the extraction yield of corresponding system.From
When the heart separates, the rotating speed of centrifuge is 5000 revs/min.
Specific process parameter and product property are shown in Table 1.
Embodiment 6
It is 2.0moldm to prepare chlorination aluminium content-3, iron tramp content is 0.17gdm-3, concentration of hydrochloric acid 1.18
mol·dm-3Liquor alumini chloridi as aqueous phase.Prepare 0.4 moldm-3N, N, N ' the N octyl group -3- oxygen glutaramides of '-four
Hexamethylene organic phase.It is standby.
Above-mentioned extraction organic phase and aqueous phase are pressed 1 respectively:1 volume ratio mixing, it is 25 DEG C to control extraction temperature, is being extracted
Stirred 0.5 hour in groove.By centrifugation, two phases were separated, and water intaking mutually determines its iron-holder, calculates the extraction yield of corresponding system.From
When the heart separates, the rotating speed of centrifuge is 5000 revs/min.
Specific process parameter and product property are shown in Table 1.
Embodiment 7
It is 2.0 moldm to prepare chlorination aluminium content-3, iron tramp content is 0.17gdm-3, concentration of hydrochloric acid 1.18
mol·dm-3Liquor alumini chloridi as aqueous phase.Prepare 0.6 moldm-3N, N, N ' the N octyl group -3- oxygen glutaramides of '-four
Hexamethylene organic phase.It is standby.
Above-mentioned extraction organic phase and aqueous phase are pressed 1 respectively:1 volume ratio mixing, it is 25 DEG C to control extraction temperature, is being extracted
Stirred 0.5 hour in groove.By centrifugation, two phases were separated, and water intaking mutually determines its iron-holder, calculates the extraction yield of corresponding system.From
When the heart separates, the rotating speed of centrifuge is 5000 revs/min.
Specific process parameter and product property are shown in Table 1.
Embodiment 8
It is 1.5 moldm to prepare chlorination aluminium content-3, iron tramp content is 8.86 × 10-3g·dm-3, concentration of hydrochloric acid is
1.18 mol·dm-3Liquor alumini chloridi as aqueous phase.Prepare 0.2 moldm-3N, N, N ' the N octyl group -3- of '-four oxygen penta 2
The hexamethylene organic phase of acid amides.It is standby.
Above-mentioned extraction organic phase and aqueous phase are pressed 1 respectively:2 volume ratio mixing, it is 25 DEG C to control extraction temperature, is being extracted
Stirred 0.5 hour in device.Mixed liquor is transferred in separator by stirring after terminating, and after stratification, aqueous phase is used into extraction
Device is taken to collect, the new organic phase for adding aqueous phase volume half continues to extract, such continuous extraction 4 times.By centrifuging two-phase
Separation, water intaking mutually determine its iron-holder, calculate the extraction yield of corresponding system.Organic phase after extraction is collected, processing to be recycled.
Specific process parameter and product property are shown in Table 2.
Embodiment 9
It is 2.0 moldm to prepare chlorination aluminium content-3, iron tramp content is 3.2 × 10-2g·dm-3, concentration of hydrochloric acid is
1.18 mol·dm-3Liquor alumini chloridi as aqueous phase.Use 0.2 moldm of back extraction recovery-3N, N, N ' N '-four are pungent
The hexamethylene organic phase of base -3- oxygen glutaramides.
Above-mentioned extraction organic phase and aqueous phase are pressed 1 respectively:2 volume ratio mixing, it is 25 DEG C to control extraction temperature, is being extracted
Stirred 0.5 hour in device.Mixed liquor is transferred in separator by stirring after terminating, and after stratification, aqueous phase is used into extraction
Device is taken to collect, the new organic phase for adding aqueous phase volume half continues to extract, such continuous extraction 4 times.By centrifuging two-phase
Separation, water intaking mutually determine its iron-holder, calculate the extraction yield of corresponding system.Organic phase after extraction is collected, processing to be recycled.
Specific process parameter and product property are shown in Table 2.
Embodiment 10
It is 2.0 moldm to prepare chlorination aluminium content-3, iron tramp content is 0.17gdm-3, concentration of hydrochloric acid 1.18
mol·dm-3Liquor alumini chloridi as aqueous phase.Prepare 0.2 moldm-3N, N, N ' the N octyl group -3- oxygen glutaramides of '-four
N-dodecane organic phase.It is standby.
Above-mentioned extraction organic phase and aqueous phase are pressed 1 respectively:2 volume ratio mixing, it is 25 DEG C to control extraction temperature, is being extracted
Stirred 0.5 hour in device.Mixed liquor is transferred in separator by stirring after terminating, and after stratification, aqueous phase is used into extraction
Device is taken to collect, the new organic phase for adding aqueous phase volume half continues to extract, such continuous extraction 4 times.By centrifuging two-phase
Separation, water intaking mutually determine its iron-holder, calculate the extraction yield of corresponding system.Organic phase after extraction is collected, processing to be recycled.
Specific process parameter and product property are shown in Table 2.
Embodiment 11
By organic 0.2 moldm for being added to liquid distributing device, adding organic phase half volume after extraction-3Sodium carbonate is molten
Liquid is mixed, and is then stirred 0.3 hour.After stratification, aqueous phase is discarded.The sodium carbonate liquor for adding same volume is carried out
Same processing, is so repeated twice.Isolated organic phase again with 2 moldm-3Hydrochloric acid solution mixing, then stir
0.3 hour.After stratification, aqueous phase is discarded.The sodium carbonate liquor for adding same volume is equally handled, and so repeatedly two
It is secondary.Isolated organic phase can reuse as new organic phase.
Extraction organic phase used in embodiment 9 is the organic phase recycled after being stripped.
Specific process parameter and product property are shown in Table 2.
The de-ferrous effect of iron content liquor alumini chloridi in above-described embodiment 1 to 10 is characterized, characterizing method is：
Visible spectrophotometry is used to embodiment 1-7, embodiment 8 to 10 is surveyed using inductively coupled plasma spectrometer
Determine the iron ion content in solution.Characterization result is shown in Tables 1 and 2.
Table 1
Table 2
Claims (4)
- A kind of 1. extracting process for preparing high-purity aluminium chloride, it is characterised in that：Utilize N, N, N ' the N octyl group -3- oxygen glutaryls of '-four Amine extracts the Fe in liquor alumini chloridi as extractant using extraction3+、Ca2+、Zn2+Impurity, extraction ability is good, can reach The standard of high-purity aluminium chloride.For extraction temperature at 20-30 DEG C, extraction time is 0.5-2 hours, H in liquor alumini chloridi+Concentration is 0.01-4 mol·dm-3, the concentration for extracting extractant in organic phase is 0.1-0.6 moldm-3, the organic phase after extraction It can be reused after back extraction recovery, extraction ability is still good.
- A kind of 2. extracting process for preparing high-purity aluminium chloride as described in claim 1, it is characterised in that：N, N, N ' N '-four are pungent Base -3- oxygen glutaramide can remove the Fe in liquor alumini chloridi as extractant3+、Ca2+、Zn2+Metal ion.
- A kind of 3. extracting process for preparing high-purity aluminium chloride as described in claim 1, it is characterised in that：Organic phase can be used for The iron and trace iron tramp of the high content in liquor alumini chloridi are extracted, the iron content in solution after extraction is less than detecting instrument Test limit.
- A kind of 4. extracting process for preparing high-purity aluminium chloride as described in claim 1, it is characterised in that：Organic phase after extraction Use 0.1-1.0 moldm-3Sodium carbonate liquor is stripped, and 1-5 moldm are used after separation-3Hydrochloric acid solution cleans, recovery Organic phase afterwards, extraction ability are still good.
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| CN103435080B (en) * | 2013-08-22 | 2015-12-09 | 中国神华能源股份有限公司 | A kind of method of aluminum chloride slurry extraction deironing |
| CN103588235B (en) * | 2013-11-18 | 2015-02-25 | 中国铝业股份有限公司 | Method for producing polyaluminium sulfate by using red mud slag |
| CN105314665B (en) * | 2014-07-16 | 2017-10-31 | 华东理工大学 | One kind compounding ferric sulfate extractant |
| KR101689960B1 (en) * | 2015-04-17 | 2017-01-03 | 주식회사 신라엔텍 | Process of preparation for recycling coagulant based on aluminium in waste purification sludge |
| CN104829481A (en) * | 2015-05-05 | 2015-08-12 | 北京科技大学 | Preparation method of N,N,N',N'-tetraoctyl-3-oxa pentanediamide |
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