CN106395874A - Method for extracting sodium chloride and aluminum chloride hexahydrate from mixed solution - Google Patents
Method for extracting sodium chloride and aluminum chloride hexahydrate from mixed solution Download PDFInfo
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- CN106395874A CN106395874A CN201610876598.XA CN201610876598A CN106395874A CN 106395874 A CN106395874 A CN 106395874A CN 201610876598 A CN201610876598 A CN 201610876598A CN 106395874 A CN106395874 A CN 106395874A
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- mixed liquor
- sodium chloride
- aluminum chloride
- salt
- 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
- C01F7/62—Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
- C01D3/08—Preparation by working up natural or industrial salt mixtures or siliceous minerals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a method for extracting sodium chloride and aluminum chloride hexahydrate from a mixed solution. The method comprises specific steps as follows: industrial alcohol is injected to a concentrated sodium chloride and aluminum chloride mixed solution firstly, the mixed solution is enabled to flow circularly and subjected to standing and solid-liquid separation, solid sodium chloride salt is obtained, the residual mixed solution is evaporated by an evaporation crystallizer and then is subjected to standing, solid-liquid separation, fresh water spraying, dehydration and drying, and solid aluminum chloride hexahydrate salt is obtained. The method has the characteristic of combining salt making modes of crystallization promotion based on industrial alcohol and crystallization based on evaporation concentration, so that sodium chloride and aluminum chloride hexahydrate can be effectively extracted from the mixed solution; the technological method is efficient, simple, and easy to operate and apply.
Description
Technical field
The present invention relates to the production technology of sodium chloride and Aluminum Chloride Hexahydrate, particularly belong to a kind of extraction chlorination from mixed liquor
Sodium and the method for Aluminum Chloride Hexahydrate.
Background technology
Gangue and flyash are the solid waste discharged in coal production and coal combustion process, its Main chemical component
Including elements such as aluminum, silicon, carbon, ferrum, calcium, magnesium.At this stage, various valuable elements have been extracted from gangue and flyash
Gradually cause the concern of every profession and trade, wherein sodium carbonate activation-hydrochloric acid leaching technique, due to simple and convenient, is that element extraction process is wide
One of technique of general employing.Hydrochloric acid leaching liquid obtained by this technique through acid adding crystallization or evaporating, concentrating and crystallizing, can obtain again
Aluminum Chloride Hexahydrate product.But, the problems of crystallization process is to employ substantial amounts of sodium carbonate because of activation stage, leads to
Hydrochloric acid leaching liquid is actually a kind of mixed liquor that also there are a large amount of sodium chloride components in addition to aluminum chloride.In addition to sodium chloride,
Some iron chloride and chlorination Calcium compounds are also contained, because their contents with chlorination al composition and sequence of crystallization are not in mixed liquor
With it is possible to be removed by the regulation and control to evaporating, concentrating and crystallizing process.However, for the aluminum chloride in mixed liquor and
Sodium chloride component, is all difficult to efficiently separate by existing technical methods such as conventional acid adding crystallization or evaporative crystallizations；This
Make to separate out along with substantial amounts of sodium chloride during Aluminum Chloride Hexahydrate crystallization, lead to the purity of Aluminum Chloride Hexahydrate product to receive very
Big impact, when serious, product purity is even less than 60%.In addition, in process of production, because the analysis of Aluminum Chloride Hexahydrate
Go out often by the way of adding hydrochloric acid or hydrogen chloride gas to promote crystallization reaction, therefore the disappearing of hydrochloric acid or hydrogen chloride gas
Consumption is also very big.
Aluminum chloride and sodium chloride, the process of these tail washings and money is all contained in the tail washings of very polymineralic hydrochloric acid leaching technique
Source is using there is also the detached technical problem of sodium chloride-aluminum chloride.According to these states of the art it may be considered that using new
Technical scheme, realizes separation and the purification of aluminum chloride and sodium chloride by the method adjusting solution chemistry component or chemical property,
And produce Aluminum Chloride Hexahydrate product.
Content of the invention
It is an object of the invention to provide a kind of method extracting sodium chloride and Aluminum Chloride Hexahydrate from mixed liquor, the method
Low production cost, the products sodium chloride being extracted and aluminum chloride purity are high.
The present invention is achieved through the following technical solutions.
The present invention is that have Matter Transfer, heating, evaporation, crystallization, liquid level or molten using commonly use in industrial crystallization production
The crystallizing evaporator of the long-pending function of measuring of liquid completes.
A kind of method extracting sodium chloride and Aluminum Chloride Hexahydrate from mixed liquor, comprises the steps：
A) mixed liquor containing sodium chloride and chlorination al composition is conveyed into crystallizing evaporator, the liquid level of record mixed liquor and
Initial volume, then starts crystallizing evaporator, controls mixeding liquid temperature between 35-85 DEG C, is evaporated and concentrates, and here
Period sampling observation, until observe solid salt crystal grain in mixed liquor；
B) determine mixeding liquid volume after concentration according to the liquid level in crystallizing evaporator, then inject quite in mixed liquor
The industrial alcohol of the purity more than 95% of mixeding liquid volume 10-55% after concentrating, in the operation bar not heated and evaporated
Mixed liquor is made to circulate 0.5-2 hour in crystallizing evaporator under part；
C) stop mixed liquor circulating in crystallizing evaporator, give off after standing 6-36 hour and be deposited on evaporation
The crystal salt of crystalliser feet, crystal salt obtains solid sodium chloride salt through centrifuge dehydration with after being dried；
D) start crystallizing evaporator and so that remaining mixed liquor is circulated in crystallizing evaporator, heat, evaporate and be dense
Contracting, controls mixeding liquid temperature between 35-85 DEG C, Al in analysis and monitoring mixed liquor3+And Na+The mass concentration of ion changes simultaneously
Ensure that the mass concentration ratio of ion maintains Al3+:Na+≥1:1.10, in the mass concentration ratio Al of ion3+:Na+Reach 1:
Crystallizing evaporator is closed during 1.10-1.20；
E) give off the tail washings part of mixed liquor in crystallizing evaporator after standing 6-36 hour, collect and take out evaporation knot
The crystal salt of brilliant device bottom deposit, after will be equivalent to concentrate in step b), the fresh water of mixeding liquid volume 2-5% is sprayed onto crystal salt
Surface, carries out centrifuge dehydration and drying to crystal salt after standing 1-3 hour, obtains the solid salt of Aluminum Chloride Hexahydrate.
In above-mentioned steps a), in described mixed liquor, the gross mass content of sodium chloride and aluminum chloride should be higher than that other impurity salts
The gross mass content of component.
In above-mentioned steps b), described industrial alcohol can also be replaced using other alcohol-based liquid such as methanol or ethanol,
Can also be replaced using ethers liquid such as the ketone liquid such as acetone or ether, can also be using alcohols, ketone, ethers liquid
Mixing liquid is replacing.
Above-mentioned steps a)-e) in, described crystallizing evaporator adopts the evaporation mode of intermittently operated, is guaranteeing accurately
Can also be using the evaporation mode of continuous operation under conditions of metering mixeding liquid volume change.
The dense salt of hydrogen chloride gas or mass concentration >=37% in above-mentioned steps d), can also be injected in described mixed liquor
Acid is to promote the crystallization of salt component.
Present invention process method is simple, easily operated, is capable of the effective of sodium chloride and chlorination al composition in mixed liquor
Separate, obtain sodium chloride and Aluminum Chloride Hexahydrate product.The tail washings finally giving off crystallizing evaporator can reclaim and again be mixed into
In initial mixed liquor, flow process of the present invention can also be discharged and continue to extract using conventional pickle liquor crystallization technique wherein each
Plant element, reach the purpose of comprehensive utilization of resources.Instant invention overcomes in existing hydrochloric acid leaching liquid between sodium chloride and aluminum chloride
It is difficult to detached technical problem, there is significant practicality and good application prospect.
Specific embodiment
To further illustrate the present invention below by specific embodiment.
Embodiment 1：
The mixed liquor being used contains sodium chloride and chlorination al composition, and wherein sodium chloride concentration is 52.01g/L, aluminum chloride
Concentration is 78.32g/L, also the impurity salt component such as calcium chloride containing the iron chloride for 6.92g/L for the concentration and concentration 3.62g/L.
In mixed liquor, the gross mass content of sodium chloride and aluminum chloride is higher than the gross mass content of other impurity salt components.
Conventional in being produced using industrial crystallization have Matter Transfer, heating, evaporation, crystallization, level gauge function
OSLO type crystallizing evaporator, using the evaporation mode of intermittently operated, comprises the steps：
A) mixed liquor containing sodium chloride and chlorination al composition is conveyed into crystallizing evaporator, the liquid level of record mixed liquor and
Initial volume, then starts crystallizing evaporator, controls mixeding liquid temperature between 80-82 DEG C, is heated, evaporated and concentrated simultaneously
Sampling observation during this period, until observe solid salt crystal grain in mixed liquor；
B) determine mixeding liquid volume after concentration according to the liquid level in crystallizing evaporator, then inject quite in mixed liquor
The industrial alcohol of the purity 96% of mixeding liquid volume 50% after concentrating, do not heated and the operating condition evaporated under make to mix
Close liquid and circulate 0.5 hour in crystallizing evaporator；
C) stop mixed liquor circulating in crystallizing evaporator, standing gives off later is deposited on evaporation knot for 6 hours
The crystal salt of brilliant device bottom, crystal salt obtains solid sodium chloride salt through centrifuge dehydration with after being dried；
D) start crystallizing evaporator and so that remaining mixed liquor is circulated in crystallizing evaporator, heat, evaporate and be dense
Contracting, controls mixeding liquid temperature between 80-82 DEG C, Al in analysis and monitoring mixed liquor3+And Na+The mass concentration of ion changes simultaneously
Ensure that the mass concentration ratio of ion maintains Al3+:Na+≥1:1.17, in the mass concentration ratio Al of ion3+:Na+Reach 1:1.17
When close crystallizing evaporator；
E) standing gives off the tail washings part of mixed liquor in crystallizing evaporator for 36 hours later, collects and take out evaporative crystallization
The crystal salt of device bottom deposit, after will be equivalent to concentrate in step b), the fresh water of mixeding liquid volume 3% is sprayed onto crystal salt surface,
Standing carried out centrifuge dehydration and drying to crystal salt after 2 hours, obtained the solid salt of Aluminum Chloride Hexahydrate.
Using as above step, the solid sodium chloride salt that every cubic metre of mixed liquor can get purity 97.26% is 18.33 thousand
Gram, the extraction ratio being equivalent to sodium chloride in mixed liquor is 34.28%；The Aluminum Chloride Hexahydrate solid salt obtaining purity 97.32% is
46.19 kilograms (24.85 kilograms of chloride containing al composition), the extraction ratio being equivalent to aluminum chloride in mixed liquor is 31.73%.Heel row
The tail washings releasing crystallizing evaporator is discharged this flow process and is continued to extract various unit therein using conventional pickle liquor crystallization technique
Element.
Embodiment 2：
Method flow is same as Example 1, and difference is that crystallizing evaporator is guaranteeing accurately to measure mixed liquor
Using the evaporation mode of continuous operation under conditions of change in volume；And finally give off in the tail washings of crystallizing evaporator, 65%
Tail liquid emissions go out flow process and using conventional pickle liquor crystallization technique continue to extract various elements therein, in addition 35% tail
Liquid reclaims and is again mixed in initial mixed liquor.
Using as above step, the solid sodium chloride salt that every cubic metre of initial mixing liquid can get purity 98.10% is
15.03 kilograms, the extraction ratio being equivalent to sodium chloride in mixed liquor is 28.35%；The Aluminum Chloride Hexahydrate obtaining purity 97.23% is solid
Body salt is 37.49 kilograms (20.15 kilograms of chloride containing al composition), and the extraction ratio being equivalent to aluminum chloride in mixed liquor is 25.02%.
Embodiment 3：
Method flow is same as Example 1, and difference is in step b) to use methanol, ethanol, the mixed liquor of acetone
Replacing industrial alcohol, this mixing liquid contains a certain amount of moisture to body, and its volume ratio is equivalent to methanol:Ethanol:Acetone:Water=
5:79:10:6；In step d), in the mixed liquor containing sodium chloride and aluminum chloride, the concentrated hydrochloric acid of implantation quality concentration 37% is to promote
Enter the crystallization of salt component, 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 every cubic metre of initial mixing liquid can get purity 98.00% is
14.26 kilograms, the extraction ratio being equivalent to sodium chloride in mixed liquor is 26.87%；The Aluminum Chloride Hexahydrate obtaining purity 95.02% is solid
Body salt is 81.16 kilograms (42.63 kilograms of chloride containing al composition), and the extraction ratio being equivalent to aluminum chloride in mixed liquor is 54.43%.
Claims (5)
1. a kind of method of extraction sodium chloride and Aluminum Chloride Hexahydrate from mixed liquor is it is characterised in that comprise the steps：
A) mixed liquor containing sodium chloride and chlorination al composition is conveyed into crystallizing evaporator, the liquid level of record mixed liquor and initial
Volume, then starts crystallizing evaporator, controls mixeding liquid temperature between 35-85 DEG C, is evaporated and concentrates, and during this period
Sampling observation, until observe solid salt crystal grain in mixed liquor；
B) determine mixeding liquid volume after concentration according to the liquid level in crystallizing evaporator, then in mixed liquor injection be equivalent to dense
The industrial alcohol of the purity more than 95% of mixeding liquid volume 10-55% after contracting, do not heated and the operating condition evaporated under
Mixed liquor is made to circulate 0.5-2 hour in crystallizing evaporator；
C) stop mixed liquor circulating in crystallizing evaporator, give off after standing 6-36 hour and be deposited on evaporative crystallization
The crystal salt of device bottom, crystal salt obtains solid sodium chloride salt through centrifuge dehydration with after being dried；
D) start crystallizing evaporator and so that remaining mixed liquor circulated in crystallizing evaporator, heat, evaporate and concentrate, control
Mixeding liquid temperature processed, between 35-85 DEG C, is analyzed and is monitored Al in mixed liquor3+And Na+The mass concentration of ion changes and ensures
The mass concentration ratio of ion maintains Al3+:Na+≥1:1.10, in the mass concentration ratio Al of ion3+:Na+Reach 1:1.10-
Crystallizing evaporator is closed when 1.20；
E) give off the tail washings part of mixed liquor in crystallizing evaporator after standing 6-36 hour, collect and take out crystallizing evaporator
The crystal salt of bottom deposit, after will be equivalent to concentrate in step b), the fresh water of mixeding liquid volume 2-5% is sprayed onto crystal salt surface,
After standing 1-3 hour, centrifuge dehydration and drying are carried out to crystal salt, obtain the solid salt of Aluminum Chloride Hexahydrate.
2. as claimed in claim 1 a kind of method extracting sodium chloride and Aluminum Chloride Hexahydrate from mixed liquor it is characterised in that
In mixed liquor described in step a), the gross mass content of sodium chloride and aluminum chloride should be higher than that the gross mass of other impurity salt components
Content.
3. as claimed in claim 1 a kind of method extracting sodium chloride and Aluminum Chloride Hexahydrate from mixed liquor it is characterised in that
Industrial alcohol described in step b) can be replaced with alcohol-based liquid, ketone liquid or ethers liquid, can also use alcohols, ketone
Replace with the mixing liquid of ethers liquid.
4. as claimed in claim 1 a kind of method extracting sodium chloride and Aluminum Chloride Hexahydrate from mixed liquor it is characterised in that
Step a)-e) described in crystallizing evaporator adopt intermittently operated evaporation mode or using continuous operation evaporation mode.
5. as claimed in claim 1 a kind of method extracting sodium chloride and Aluminum Chloride Hexahydrate from mixed liquor it is characterised in that
The knot to promote salt component for the concentrated hydrochloric acid of injection hydrogen chloride gas or mass concentration >=37% in mixed liquor described in step d)
Brilliant.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610876598.XA CN106395874B (en) | 2016-10-08 | 2016-10-08 | A kind of method that sodium chloride and Aluminum Chloride Hexahydrate are extracted from mixed liquor |
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| CN201610876598.XA CN106395874B (en) | 2016-10-08 | 2016-10-08 | A kind of method that sodium chloride and Aluminum Chloride Hexahydrate are extracted from mixed liquor |
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| CN106395874B CN106395874B (en) | 2017-08-25 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108225968A (en) * | 2017-12-27 | 2018-06-29 | 四川峨胜水泥集团股份有限公司 | The assay method of urea content in a kind of NOx reducing agent aqueous solution of urea |
| CN113149035A (en) * | 2020-12-29 | 2021-07-23 | 中国科学院生态环境研究中心 | Method for treating waste sodium chloride salt |
| CN113511661A (en) * | 2021-06-30 | 2021-10-19 | 孝感广盐华源制盐有限公司 | Method for producing edible salt by using salt production waste liquid |
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|---|---|---|---|---|
| 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 CN201610876598.XA patent/CN106395874B/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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108225968A (en) * | 2017-12-27 | 2018-06-29 | 四川峨胜水泥集团股份有限公司 | The assay method of urea content in a kind of NOx reducing agent aqueous solution of urea |
| CN113149035A (en) * | 2020-12-29 | 2021-07-23 | 中国科学院生态环境研究中心 | Method for treating waste sodium chloride salt |
| CN113511661A (en) * | 2021-06-30 | 2021-10-19 | 孝感广盐华源制盐有限公司 | Method for producing edible salt by using salt production waste liquid |
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