CN106430268A - Method of extracting high-purity aluminum chloride hexahydrate from mixed liquid - Google Patents
Method of extracting high-purity aluminum chloride hexahydrate from mixed liquid Download PDFInfo
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- CN106430268A CN106430268A CN201610876616.4A CN201610876616A CN106430268A CN 106430268 A CN106430268 A CN 106430268A CN 201610876616 A CN201610876616 A CN 201610876616A CN 106430268 A CN106430268 A CN 106430268A
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- mixed liquor
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- crystallizing evaporator
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention provides a method of extracting high-purity aluminum chloride hexahydrate from mixed liquid. The method specifically includes: concentrating the mixed liquid containing aluminum chloride, a sodium chloride, calcium chloride and iron chloride, continuing to evaporate away water equivalent to 20-50% of volume at the time when salt starts to be separated out; adding industrial alcohol, enabling part of solid-phase salt which is separated out, and evaporating and crystallizing the rest mixed liquid after mixing, standing and solid-liquid separating; performing standing, solid-liquid separating, fresh water spraying, dewatering and drying to obtain high-purity aluminum chloride hexhydrate solid salt. The method has the advantages that a mode of solvent regulation and recrystallization is utilized to effectively separate aluminum chloride hexahydrate out of the mixed liquid, and the method is efficient, simple and easy to operate and apply.
Description
Technical field
The present invention relates to the production technology of Aluminum Chloride Hexahydrate, particularly belong to one from mixed liquor, extract high-purity six water chlorinations
The method of aluminium.
Background technology
Gangue and flyash are the solid waste producing in the production of coal and coal combustion process, its primary chemical group
It is divided into Al2O3、SiO2、Fe2O3、CaO、MgO、TiO2Deng, and wherein Al2O3Content general all more than 40%.In recent years, from
Gangue and flyash extract aluminum oxide caused researcher and pay close attention to widely, in order to improve the dissolution of wherein aluminium
Rate, after utilizing sodium carbonate activation, hydrochloric acid leaching becomes flyash and gangue puies forward one of widely used technique of aluminium.This technique obtains
The method that the pickle liquor arrived generally can pass through enriching salt acid crystal or evaporative crystallization, can obtain Aluminum Chloride Hexahydrate product.But
It is, owing to activation stage introduces substantial amounts of sodium carbonate, to cause in hydrochloric acid leaching liquid in addition to containing aluminium chloride, possibly together with greatly
The sodium chloride of amount and partial oxidation iron and calcium chloride, wherein calcium chloride and iron chloride are owing to content is low and sequence of crystallization and chlorination
Aluminium difference, therefore can be removed by the regulation and control to evaporating, concentrating and crystallizing process.But, for aluminium chloride and chlorine
Changing sodium, being all difficult to efficiently separate by existing technical methods such as conventional acid adding crystallization or evaporative crystallizations, this results in
Separating out along with substantial amounts of sodium chloride during Aluminum Chloride Hexahydrate crystallization, the purity causing Aluminum Chloride Hexahydrate product is seriously low
In industrial standard.Additionally, owing to usually needing to add concentrated hydrochloric acid or being passed through hydrogen chloride gas in the production process of Aluminum Chloride Hexahydrate
Body promotes the carrying out of crystallization, and therefore production cost is also bigger.
Generally all exist in the production process of the acid technological process of Aluminum Chloride Hexahydrate Aluminum Chloride Hexahydrate and sodium chloride and its
The separation problem of his impurity, and it is more difficult to obtain high-purity Aluminum Chloride Hexahydrate.According to these states of the art, it may be considered that use
New technical scheme, the method for condensing crystallizing rate and chemical property by controlling solution removes sodium chloride as impurity, and produces height
Pure Aluminum Chloride Hexahydrate product.
Content of the invention
It is an object of the invention to provide a kind of method extracting high-purity Aluminum Chloride Hexahydrate from mixed liquor, the method produces
Low cost, the product Aluminum Chloride Hexahydrate purity extracted is high.
The present invention is achieved through the following technical solutions.
The present invention is to utilize that commonly uses in industrial crystallization production to have Matter Transfer, heating, evaporation, crystallization, liquid level or molten
Liquid amasss what the crystallizing evaporator of function of measuring completed.
A kind of method extracting high-purity Aluminum Chloride Hexahydrate from mixed liquor, comprises the steps：
A) in crystallizing evaporator, the mixed liquor containing aluminium chloride, sodium chloride, calcium chloride and iron chloride is added, according to mixing
Its initial volume of the liquid level recorder of liquid, then starts crystallizing evaporator, controls the temperature of mixed liquor entering between 35-85 DEG C
, until there is grain of salt crystals in mixed liquor in row evaporation operation, during this period constantly sampling detection；
B) determine mixeding liquid volume now according to the liquid level of crystallizing evaporator, then proceed to evaporate and be equivalent to now
The water yield of mixeding liquid volume 20%-50%, occurs in making crystallizing evaporator that crystal salt precipitates and concentrates mixed liquor；
C) according to the liquid level of crystallizing evaporator determine crystal salt precipitate and concentrate mixed liquor cumulative volume, stop heating and
Evaporation operation, and addition is equivalent to crystal salt precipitation and concentration mixed liquor cumulative volume 10-55%, concentration exist in concentration mixed liquor
The industrial alcohol of more than 95%, makes concentration mixed liquor circulate 0.5-2 hour in crystallizing evaporator, and makes part crystallization
Salt precipitation is dissolved again again；
D) stop concentration mixed liquor circulates and stands 6-36 hour, then will be deposited on bottom crystallizing evaporator
Crystal salt is discharged, and crystal salt is through centrifugal dehydration and obtains solid sodium chloride salt after being dried；
E) determine the volume of concentration mixed liquor according to the liquid level in crystallizing evaporator, start crystallizing evaporator and simultaneously continue evaporation
Falling to be equivalent to the water yield of its volume 10%-40%, period keeps concentrating mixed liquor circulating in crystallizing evaporator, controls
Concentration mixeding liquid temperature, between 35-85 DEG C, is then shut off crystallizing evaporator；
F) concentrate mixed liquor after standing 6-36 hour, to discharge the supernatant in crystallizing evaporator, isolate crystallizing evaporator
The crystal salt of bottom precipitation, will be equivalent to crystal salt precipitation and the fresh water sprinkling concentrating mixed liquor cumulative volume 2-5% in step c)
It to crystal salt surface, is centrifuged being dehydrated and dry to crystal salt after standing 1-3 hour, obtains consolidating of high-purity Aluminum Chloride Hexahydrate
Body salt.
In above-mentioned steps a), in described mixed liquor, the gross mass content of sodium chloride and aluminium chloride should be other impurity salt groups
Divide gross mass content more than 5 times.
In above-mentioned steps c), described industrial alcohol can also use other alcohol-based liquid such as methyl alcohol or ethanol to replace,
Can also use the ethers liquid such as ketone liquid or ether such as acetone to replace, alcohols, ketone, ethers liquid can also be used
Mixing liquid replaces.
Above-mentioned steps a)-f) in, the evaporation mode of described crystallizing evaporator uses the mode of intermittently operated, is guaranteeing
Also the mode of continuous operation can be used under conditions of enough accurately metering mixeding liquid volume changes.
In above-mentioned steps e), described concentration can also inject hydrogen chloride gas or mass concentration >=37% in mixed liquor
Concentrated hydrochloric acid is to promote the crystallization of salt component.
Present invention process method is simple, easily operated and production cost is relatively low, can be by sodium chloride in mixed liquor and chlorination
Al composition efficiently separates, and finally gives high-purity Aluminum Chloride Hexahydrate product more than 98% for the purity.Last crystallizing evaporator
In tail washings can rejoin in initial mixed liquor, reach the purpose of resources circulation and comprehensive utilization.Present invention achieves
Separate the technical problem of high-purity Aluminum Chloride Hexahydrate from existing hydrochloric acid leaching liquid mixture system, there is significant practicality and very well
Application prospect.
Detailed description of the invention
Further illustrate the present invention below by specific embodiment.
Embodiment 1
A kind of method extracting high-purity Aluminum Chloride Hexahydrate from mixed liquor：
The mixed liquor being used contains sodium chloride and aluminium chloride component, and wherein sodium chloride concentration is 52.01g/L, aluminium chloride
Concentration is 78.32g/L, possibly together with the impurity salt component such as calcium chloride of the iron chloride that concentration is 6.92g/L and concentration 3.62g/L.
In mixed liquor, the gross mass content of sodium chloride and aluminium chloride is 12.37 times of other impurity salt component gross mass content.
Utilize that industrial crystallization is conventional in producing has Matter Transfer, heating, evaporation, crystallization, level gauge function
OSLO type crystallizing evaporator, uses the evaporation mode of intermittently operated, comprises the steps：
A) in crystallizing evaporator, the mixed liquor containing aluminium chloride, sodium chloride, calcium chloride and iron chloride is added, according to mixing
Its initial volume of the liquid level recorder of liquid, then starts crystallizing evaporator, controls the temperature of mixed liquor entering between 82-85 DEG C
, until there is grain of salt crystals in mixed liquor in row evaporation operation, during this period constantly sampling detection；
B) determine mixeding liquid volume now according to the liquid level of crystallizing evaporator, then proceed to evaporate and be equivalent to now
The water yield of mixeding liquid volume 45%, occurs in making crystallizing evaporator that crystal salt precipitates and concentrates mixed liquor；
C) according to the liquid level of crystallizing evaporator determine crystal salt precipitate and concentrate mixed liquor cumulative volume, stop heating and
Evaporation operation, and be equivalent to crystal salt precipitation and concentrate mixed liquor cumulative volume the 55%th, concentration exist to concentrating mixed liquor adds
The industrial alcohol of 96%, makes concentration mixed liquor circulate in crystallizing evaporator 1.5 hours, and makes a part of crystal salt precipitate
Again again dissolve；
D) stop concentration mixed liquor circulates and stands 36 hours, then will be deposited on the knot bottom crystallizing evaporator
Brilliant salt is discharged, and crystal salt is through centrifugal dehydration and obtains solid sodium chloride salt after being dried；
E) determine the volume of concentration mixed liquor according to the liquid level in crystallizing evaporator, start crystallizing evaporator and simultaneously continue evaporation
Falling to be equivalent to the water yield of its volume 40%, period keeps concentrating mixed liquor circulating in crystallizing evaporator, controls concentration
Mixeding liquid temperature, between 82-85 DEG C, is then shut off crystallizing evaporator；
F) concentrate mixed liquor after standing 36 hours, to discharge the supernatant in crystallizing evaporator, isolate at the bottom of crystallizing evaporator
The crystal salt of portion's precipitation, the fresh water that will be equivalent to crystal salt precipitation and concentration mixed liquor cumulative volume 5% in step c) is sprayed onto knot
Brilliant salt surface, is centrifuged dehydration and is dried, obtaining the solid salt of high-purity Aluminum Chloride Hexahydrate to crystal salt after standing 3 hours.
Using as above step, the solid sodium chloride salt that the mixed liquor of every cubic metre can get purity 98.25% is 40.74 thousand
Gram, the recovery rate being equivalent to sodium chloride in mixed liquor is 76.97%；The Aluminum Chloride Hexahydrate solid salt obtaining purity 99.92% is
51.22 kilograms (chloride containing al composition 28.29 kilograms), the recovery rate being equivalent to aluminium chloride in mixed liquor is 35.88%.Heel row
The tail washings releasing crystallizing evaporator is discharged this flow process and uses conventional acid immersion liquid crystallization technique to continue to extract various unit therein
Element.
Embodiment 2
Method flow is same as in Example 1, and difference is that crystallizing evaporator is guaranteeing accurately to measure mixed liquor
The evaporation mode of continuous operation is used under conditions of Volume Changes；And finally give off in the tail washings of crystallizing evaporator, 50%
Tail liquid emissions go out flow process and use conventional acid immersion liquid crystallization technique to continue to extract various element therein, the tail of other 50%
Liquid reclaims and is again mixed in initial mixed liquor.
Using as above step, the solid sodium chloride salt that the initial mixing liquid of every cubic metre can get purity 97.85% is
42.01 kilograms, the recovery rate being equivalent to sodium chloride in mixed liquor is 79.04%；The Aluminum Chloride Hexahydrate obtaining purity 99.94% is solid
Body salt is 50.05 kilograms (chloride containing al compositions 27.67 kilograms), and the recovery rate being equivalent to aluminium chloride in mixed liquor is 34.34%.
Embodiment 3
Method flow is same as in Example 1, and difference is in step c) to use methyl alcohol, ethanol, the mixed liquor of acetone
Body replaces industrial alcohol, and this mixing liquid contains a certain amount of moisture, and its volume ratio is equivalent to methyl alcohol:Ethanol:Acetone:Water=
5:79:10:6；In step e), in the mixed liquor containing sodium chloride and aluminium chloride, the concentrated hydrochloric acid of implantation quality concentration 37% is to promote
Entering the crystallization of Aluminum Chloride Hexahydrate, the injected slurry volume amount of concentrated hydrochloric acid is equivalent to the 1/3 of now mixeding liquid volume.
Using as above step, the solid sodium chloride salt that the initial mixing liquid of every cubic metre can get purity 98.30% is
41.46 kilograms, the recovery rate being equivalent to sodium chloride in mixed liquor is 78.37%；The Aluminum Chloride Hexahydrate obtaining purity 99.91% is solid
Body salt is 90.24 kilograms (chloride containing al compositions 49.84 kilograms), and the recovery rate being equivalent to aluminium chloride in mixed liquor is 63.20%.
Claims (5)
1. the method extracting high-purity Aluminum Chloride Hexahydrate from mixed liquor, it is characterised in that comprise the steps：
A) in crystallizing evaporator, the mixed liquor containing aluminium chloride, sodium chloride, calcium chloride and iron chloride is added, according to mixed liquor
Its initial volume of liquid level recorder, then starts crystallizing evaporator, controls the temperature of mixed liquor and steaming between 35-85 DEG C
Send out operation, during this period constantly sampling detection, until grain of salt crystals occurs in mixed liquor；
B) determine mixeding liquid volume now according to the liquid level of crystallizing evaporator, then proceed to evaporate and be equivalent to now mix
Liquid amasss the water yield of 20%-50%, occurs that crystal salt precipitates and concentrates mixed liquor in making crystallizing evaporator；
C) determine that crystal salt precipitates and concentrates the cumulative volume of mixed liquor according to the liquid level of crystallizing evaporator, stop heating and evaporation
Operation, and be equivalent to crystal salt precipitation to concentrating mixed liquor adds and concentrate mixed liquor cumulative volume 10-55%, concentration 95%
Above industrial alcohol, makes concentration mixed liquor circulate 0.5-2 hour in crystallizing evaporator, and makes a part of crystal salt sink
Form sediment and again again dissolve；
D) stop concentration mixed liquor circulates and stands 6-36 hour, then will be deposited on the crystallization bottom crystallizing evaporator
Salt is discharged, and crystal salt is through centrifugal dehydration and obtains solid sodium chloride salt after being dried；
E) determine the volume of concentration mixed liquor according to the liquid level in crystallizing evaporator, start crystallizing evaporator and simultaneously continue to evaporate phase
When in the water yield of its volume 10%-40%, period keeps concentrating mixed liquor circulating in crystallizing evaporator, controls concentration
Mixeding liquid temperature, between 35-85 DEG C, is then shut off crystallizing evaporator；
F) concentrate mixed liquor after standing 6-36 hour, to discharge the supernatant in crystallizing evaporator, isolate bottom crystallizing evaporator
The crystal salt of precipitation, the fresh water that will be equivalent to crystal salt precipitation and concentration mixed liquor cumulative volume 2-5% in step c) is sprayed onto knot
Brilliant salt surface, is centrifuged being dehydrated and dry to crystal salt after standing 1-3 hour, obtains the solid of high-purity Aluminum Chloride Hexahydrate
Salt.
2. a kind of method extracting high-purity Aluminum Chloride Hexahydrate from mixed liquor as claimed in claim 1, it is characterised in that step
A) in the mixed liquor described in, the gross mass content of sodium chloride and aluminium chloride should be 5 times of other impurity salt component gross mass content
Above.
3. a kind of method extracting high-purity Aluminum Chloride Hexahydrate from mixed liquor as claimed in claim 1, it is characterised in that step
C) the industrial alcohol methyl alcohol described in, ethanol or acetone substitute, or replace with their mixing liquid.
4. a kind of method extracting high-purity Aluminum Chloride Hexahydrate from mixed liquor as claimed in claim 1, it is characterised in that step
A)-f) described in crystallizing evaporator evaporation mode use intermittently operated mode or employing continuous operation mode.
5. a kind of method extracting high-purity Aluminum Chloride Hexahydrate from mixed liquor as claimed in claim 1, it is characterised in that step
E) concentrated hydrochloric acid concentrating injection hydrogen chloride gas or mass concentration >=37% in mixed liquor described in is to promote the knot of salt component
Brilliant.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610876616.4A CN106430268B (en) | 2016-10-08 | 2016-10-08 | A kind of method that high-purity Aluminum Chloride Hexahydrate is extracted from mixed liquor |
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|---|---|---|---|
| CN201610876616.4A CN106430268B (en) | 2016-10-08 | 2016-10-08 | A kind of method that high-purity Aluminum Chloride Hexahydrate is extracted from mixed liquor |
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| CN106430268B CN106430268B (en) | 2017-10-17 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6241958B1 (en) * | 1991-06-27 | 2001-06-05 | Metallgesellschaft Aktiengesellschaft | Process for preparing sulfate-containing basic solutions of polyaluminumchloride |
| CN102574022A (en) * | 2009-06-25 | 2012-07-11 | 弗拉克普尔控股有限责任公司 | Method of making pure salt from frac-water/wastewater |
| CN103979590A (en) * | 2014-05-19 | 2014-08-13 | 中国神华能源股份有限公司 | High-purity crystalline aluminum chloride preparation method |
| CN104743583A (en) * | 2015-04-24 | 2015-07-01 | 傅培鑫 | Method for producing potassium sulphate and aluminium chloride by utilizing potassium alum |
| CN104773746A (en) * | 2014-01-14 | 2015-07-15 | 贵阳铝镁设计研究院有限公司 | Anhydrous aluminum chloride production method |
-
2016
- 2016-10-08 CN CN201610876616.4A patent/CN106430268B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6241958B1 (en) * | 1991-06-27 | 2001-06-05 | Metallgesellschaft Aktiengesellschaft | Process for preparing sulfate-containing basic solutions of polyaluminumchloride |
| CN102574022A (en) * | 2009-06-25 | 2012-07-11 | 弗拉克普尔控股有限责任公司 | Method of making pure salt from frac-water/wastewater |
| CN104773746A (en) * | 2014-01-14 | 2015-07-15 | 贵阳铝镁设计研究院有限公司 | Anhydrous aluminum chloride production method |
| CN103979590A (en) * | 2014-05-19 | 2014-08-13 | 中国神华能源股份有限公司 | High-purity crystalline aluminum chloride preparation method |
| CN104743583A (en) * | 2015-04-24 | 2015-07-01 | 傅培鑫 | Method for producing potassium sulphate and aluminium chloride by utilizing potassium alum |
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