CN106830029A - A kind of potassium aluminate solution crystal seed decomposes the process of production aluminium hydroxide - Google Patents
A kind of potassium aluminate solution crystal seed decomposes the process of production aluminium hydroxide Download PDFInfo
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- CN106830029A CN106830029A CN201710000642.5A CN201710000642A CN106830029A CN 106830029 A CN106830029 A CN 106830029A CN 201710000642 A CN201710000642 A CN 201710000642A CN 106830029 A CN106830029 A CN 106830029A
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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
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
- C01F7/144—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by precipitation due to cooling, e.g. as part of the Bayer process
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The present invention relates to alkaline media field of hydrometallurgy, specifically a kind of potassium aluminate solution crystal seed decomposes the process of production aluminium hydroxide, comprises the following steps：A, aluminic acid potassium solution is poured into reactor, in 200 280g/L, solution caustic ratio is 1.35 1.75 for alkali concn control, and opens water-bath circulation and stir, control decompose just temperature between 60 90 DEG C；B, in system add aluminium hydroxide crystal seed, stirring decompose, crystal seed coefficient be 0.5 4.0, stir speed (S.S.) be 100 500rpm；C, decomposing solution is cooled to 40 50 DEG C, after decomposition of crystal seed reaction terminating, stops water-bath circulation and stir, be separated by filtration and obtain seed precipitation solution and aluminum hydroxide product.Under the operating condition of the inventive method, resolution ratio up to 70%, far above the decomposition of crystal seed efficiency of traditional sodium aluminate system 55%, while product purity is high, pattern is good, particle size is big.
Description
Technical field
It is a kind of potassium aluminate lyotropic liquid crystal specifically the present invention relates to field of aluminum oxide production in alkaline media hydrometallurgy
Plant the process for decomposing production aluminium hydroxide.
Background technology
Potassium resource can be divided into water-soluble potassium resource and water-insoluble potassium resource, global explored water-soluble potassium resource industry
Reserves are in 20,000,000,000 tons of K2More than O, but be distributed not perfectly flat weighing apparatus, more than 90% reserves are mainly distributed on Canada, Russia, white
The countries such as Russia, France, Germany, the U.S., Israel, Jordan, and grade is higher.And in most of development such as Asia, Latin America
Countries and regions, sylvite reserves are little, and grade is relatively low.Comparatively, water-insoluble potassium ore resources enrich and are distributed wide very much
General, all kinds of potassium bearing rocks based on potassium feldspar, kalunite etc. are distributed in the whole world, but are difficult to industrial utilization at present.Together
Shi Quanqiu alum clay ore reserves has 28,000,000,000 tons altogether, and non-bauxitic such as nepheline, alum are reasonably comprehensively utilized in aluminum i ndustry production
Stone, flyash etc., there is realistic meaning.
At present, the decomposition of crystal seed research on aluminate solution is mainly reflected in system containing sodium, i.e. predominantly sodium aluminate solution
The decomposition of crystal seed research of liquid, and pair seldom reported with the decomposition of crystal seed of aluminic acid potassium solution.The decomposition of crystal seed of aluminate solution is always
It is that Bayer process produces one critical process of aluminium hydroxide, but there is also that Disassembling Products rate is low, the resolving time is long, seed simultaneously
Than it is big, product granularity is small the problems such as.Show that its major influence factors includes decomposition temperature, molten for the research of decomposition of crystal seed process
Liquid caustic ratio, caustic sodium concentration, seed ratio and stir speed (S.S.) etc..Decomposition of crystal seed temperature is raised, is conducive to the agglomeration of crystal, together
When temperature higher be also beneficial to growing up for crystal, so as to obtain the product that granularity is big, impurity is few, but the rising of temperature is also anticipated
Taste the reduction of the degree of supersaturation of solution and the reduction of decomposition rate, while also increasing energy consumption；With decomposition stoste Crater corrosion
Value is reduced, and the decomposition rate of solution, resolution ratio and production capacity are significantly improved, but the requirement of simultaneously low molecular proportion to a upper operation
It is higher and be also easy to produce more fine graineds；The stoste of medium caustic sodium concentration is least stablized, and decomposition rate is very fast, but also implies that low
Output capacity and production capacity；The crystal seed that early stage is added is being decomposed, fine grained crystal seed easily occurs agglomeration, and coarse granule crystal seed is then simple crystalline substance
Body grows, and fine grained crystal seed and the fast speed of growth are beneficial to crystal growth, and crystal seed amount is beneficial to the generation of agglomeration bulky grain less, therefore
The large or fine granule and proper amount of crystal seed amount for choosing proper ratio are important；Crystal keeps during appropriate stirring can make solution
Suspended state, contacts well with solution, and composition is uniform, while being conducive to the uniform of crystal to grow up.The studies above is based on sodium system
Aluminate solution, therefore also need further research for the decomposition of potassium aluminate solution crystal seed.
The content of the invention
It is an object of the invention to provide the process that a kind of potassium aluminate solution crystal seed decomposes production aluminium hydroxide.It is based on
Domestic further severe potassium resource shortage problem, urgent need carries out height to the water-insoluble aluminum ore containing potassium such as such as alunite, potassium feldspar
The comprehensive utilization of cleaning is imitated, separated again to the treatment of such phosphate-containing ore to can obtain potassium aluminate molten by alkaline media hydrometallurgy
Liquid, implementing decomposition of crystal seed to such aluminic acid potassium solution can obtain the controllable aluminum hydroxide product of pattern granularity.
The first aspect of the present invention, there is provided a kind of potassium aluminate solution crystal seed decomposes the process of production aluminium hydroxide, bag
Include following steps：
A, aluminic acid potassium solution is poured into reactor, alkali concn is (with K2O is counted) control in 200-280g/L, solution Crater corrosion
It is 1.35-1.75 to be worth, and opens water-bath circulation and stir, so that solution temperature and even concentration, just temperature exists for control decomposition
Between 60-90 DEG C；
B, in system add aluminium hydroxide crystal seed, stirring decompose, crystal seed coefficient be 0.5-4.0, stir speed (S.S.) is 100-
500rpm；
C, decomposing solution is cooled to 40-50 DEG C, after decomposition of crystal seed reaction terminating, stops water-bath circulation and stir, pass through
Filter isolated seed precipitation solution and product.
Decompose initial temperature lower, because degree of supersaturation is big, solution resolution ratio is higher；Initial temperature is higher, beneficial to fine grain crystal
Agglomeration, corresponding product granularity increases.Equally, end temperature is low also beneficial to decomposing, and beneficial to crystal growth, product is thicker, but product granularity
Polarization, is unfavorable for product homogeneity.Therefore selection temperature schedule is between 60-90 DEG C of initial temperature, end is warm 40-50 DEG C.
Crystal seed coefficient is high, and the resolution ratio of aluminic acid potassium solution can be improved due to the surface of the seed product high, and crystal can be promoted to give birth to
It is long, obtain coarse granule product, but too high seed, than making the intensity decreases of product, comprehensive selection seed ratio is 0.5-4.0.
Stir speed (S.S.) usury promotes the decomposition reaction of seed surface in the mass transfer of solution, crystal seed is fully contacted with solution,
But too high stir speed (S.S.) can cause the abrasion of crystal seed and crush, it is unfavorable for producing coarse granule aluminium hydroxide.Therefore selection stirring speed
Rate is in 200-600rpm.
Alkali concn is high, causes solution degree of supersaturation low, is unfavorable for crystal agglomeration, and product granularity is smaller；Alkali concn reduction, it is molten
The equilibrium concentration of aluminum oxide is decreased in liquid, and decomposition rate is significantly accelerated, and resolution ratio is also accordingly improved, but alkali concn is low,
The equilibrium concentration of aluminum oxide is too low, the aluminium hydroxide yield reduction of unit volume.
Under conditions of decomposing initial temperature and decomposing end temperature necessarily, rate of temperature fall embodies the reaction time of decomposition of crystal seed.
Initial decomposition, reaction rate changes with time substantially, and into after the reaction later stage, the change for changing over time resolution ratio is failed to understand
It is aobvious, so it needs to be determined that the suitable reaction time.Therefore selection rate of temperature fall is 0.5-2 DEG C/h.
Preferably, just temperature is 70 DEG C to the decomposition in described step A.
Preferably, the alkali concn in the step A be 240g/L, caustic ratio be 1.4.
Preferably, the decomposition temperature control stabilization in the step B is at 60-90 DEG C.
Preferably, the crystal seed coefficient in described step B is 2.
Preferably, the stir speed (S.S.) in described step B is 200rpm.
Preferably, the rate of temperature fall in described step C is controlled in 0.5-2 DEG C/h.
Preferably, the decomposing solution in described step C is cooled to 40 DEG C.
The present invention provides a kind of decomposition of crystal seed method of aluminic acid potassium solution, based on further severe potassium resource problem, is badly in need of
The comprehensive utilization of high-efficiency cleaning is carried out to such as water-insoluble potassium resource such as alunite, potassium feldspar containing potassium, aluminum ore, by alkaline media
Treatment of the hydrometallurgy to such phosphate-containing ore can obtain aluminic acid potassium solution through later separation again, and such aluminic acid potassium solution is implemented
Potassium aluminium lock out operation is extremely crucial as decomposition of crystal seed.This method uses decomposition temperature to be down to last temperature by 60-90 DEG C of initial temperature
40-50 DEG C, alkali concn is (with K2O is counted) in 200-280g/L, solution caustic ratio is 1.35-1.75, and crystal seed coefficient is for control
0.5-4.0, stir speed (S.S.) is 100-500rpm, and the resolving time is controlled in 24-72h.By under the operating condition of as above technique,
Resolution ratio not only can reach more than 70%, the decomposition of crystal seed efficiency much larger than the 55% of traditional sodium system, while product purity is high, shape
Looks are good, particle size is big.The inventive method uses and adds aluminium hydroxide crystal seed to realize the knot of aluminium hydroxide to aluminic acid potassium solution
Partial crystallization goes out, and process conditions are simply easily manipulated, and has certain reference role for the decomposition of crystal seed of potassium system aluminate solution, and
The aluminum hydroxide product of energy high yield, expeditiously output high-purity, there is preferable economy and practicality.
Compared with prior art, the invention has the advantages that：
1st, the resolution ratio that not additivated potassium aluminate solution crystal seed is decomposed in the method for the present invention is higher than sodium system, can
More than 70% is reached, the decomposition of crystal seed efficiency much larger than the 55% of traditional sodium system, while product purity is high, pattern is good, particle chi
It is very little big.
2nd, due to K in the method for the present invention+Radius ratio Na+Radius is big, makes it be more difficult to account for Al (OH)3H in lattice dot matrix+'s
Position, therefore it is less to decomposite impurity such as lattice alkali etc. in the aluminium hydroxide for coming from aluminic acid potassium solution.
Brief description of the drawings
Fig. 1 is aluminum hydroxide product XRD prepared by present invention process.
Fig. 2 is aluminum hydroxide product scanning electron microscope (SEM) photograph prepared by present invention process.
Specific embodiment
The specific embodiment that the present invention is provided is elaborated with reference to embodiment.
Embodiment 1
Step (1)：By alkali concn (with K2O is counted) for 240g/L, the aluminic acid potassium solution that caustic ratio is 1.4 or so are poured into instead
In answering device, and open water-bath circulation and stir, so that solution temperature and even concentration, it is 70 DEG C control to decompose just temperature, is opened
Begin to add aluminium hydroxide crystal seed, seed ratio is that crystal seed coefficient elects 2 as, and stir speed (S.S.) elects 200rpm as.
Step (2)：In decomposition of crystal seed course of reaction, rate of temperature fall is controlled in 0.5-2 DEG C/h, it is ensured that reaching optimal point
Solution yield and speed, while sampling 20ml every 5 hours, after being centrifuged, take supernatant liquor sampling analysis potassium oxide and oxygen
Change aluminium content, lower floor's solids of sedimentation is dried after 2-5 times is washed with hot deionized water, and drying temperature is about 80 DEG C, then carries out solid slag X
X ray diffractometer x material phase analysis and ESEM morphology analysis.
Step (3)：Decomposing solution is cooled to 40 DEG C, after decomposition of crystal seed reaction terminating, is stopped water-bath circulation and is stirred, warp
It is separated by filtration and obtains seed precipitation solution and product, analyze potassium oxide and alumina content in final mother liquor, while weighs final producing
Quality draws the resolution ratio of whole process；Result shows final resolution ratio up to 75%, solid phase X-ray diffractometer material phase analysis with
Show that product is high-purity aluminum hydroxide particles after ESEM morphology analysis, surface topography physically well develop and particle size compared with
Greatly.Product X-ray diffractometer is with ESEM result as depicted in figs. 1 and 2.
Below the preferred embodiment to the invention is illustrated, but the invention be not limited to it is described
Embodiment, those of ordinary skill in the art can also make a variety of equivalent on the premise of without prejudice to the invention spirit
Modification or replacement, these equivalent modifications or replacement are all contained in the application claim limited range.
Claims (8)
1. a kind of potassium aluminate solution crystal seed decomposes the process of production aluminium hydroxide, it is characterised in that comprise the following steps：
A, aluminic acid potassium solution is poured into reactor, alkali concn is with K2In 200-280g/L, solution caustic ratio is for O meter controls
1.35-1.75, and open water-bath circulation and stir, control decomposes first temperature between 60-90 DEG C；
B, in system add aluminium hydroxide crystal seed, stirring decompose, crystal seed coefficient be 0.5-4.0, stir speed (S.S.) is 100-
500rpm；
C, decomposing solution is cooled to 40-50 DEG C, after decomposition of crystal seed reaction terminating, stops water-bath circulation and stir, through filtering point
From obtaining seed precipitation solution and aluminum hydroxide product.
2. potassium aluminate solution crystal seed according to claim 1 decomposes the process of production aluminium hydroxide, it is characterised in that
Just temperature is 70 DEG C for decomposition in the step A.
3. potassium aluminate solution crystal seed according to claim 1 decomposes the process of production aluminium hydroxide, it is characterised in that
Alkali concn in the step A is with K2It is 1.4 that O is calculated as 240g/L, caustic ratio.
4. potassium aluminate solution crystal seed according to claim 1 decomposes the process of production aluminium hydroxide, it is characterised in that
Decomposition temperature control stabilization in the step B is at 60-90 DEG C.
5. potassium aluminate solution crystal seed according to claim 1 decomposes the process of production aluminium hydroxide, it is characterised in that
Crystal seed coefficient in the step B is 2.
6. potassium aluminate solution crystal seed according to claim 1 decomposes the process of production aluminium hydroxide, it is characterised in that
Stir speed (S.S.) in the step B is 200rpm.
7. potassium aluminate solution crystal seed according to claim 1 decomposes the process of production aluminium hydroxide, it is characterised in that
Rate of temperature fall in the step C is controlled in 0.5-2 DEG C/h.
8. potassium aluminate solution crystal seed according to claim 1 decomposes the process of production aluminium hydroxide, it is characterised in that
Decomposing solution in the step C is cooled to 40 DEG C.
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| CN201710000642.5A CN106830029B (en) | 2017-01-03 | 2017-01-03 | A kind of potassium aluminate solution crystal seed decomposes the process of production aluminium hydroxide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107265487A (en) * | 2017-06-15 | 2017-10-20 | 郑州中绿环保新材料有限公司 | A kind of method that use solid sodium aluminate produces special aluminium hydroxide product |
| CN112028095A (en) * | 2020-08-12 | 2020-12-04 | 中铝山东有限公司 | Superfine aluminum hydroxide seed crystal and preparation method thereof, submicron aluminum hydroxide and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4562059A (en) * | 1984-06-08 | 1985-12-31 | Chiyoda Chemical Engineering & Construction Co., Ltd. | Method of preparing alumina |
| JPH07126011A (en) * | 1993-10-26 | 1995-05-16 | Showa Denko Kk | Method for crystallizing columnar aluminum hydroxide |
| CN101391792A (en) * | 2008-11-11 | 2009-03-25 | 中国铝业股份有限公司 | Method for preparing acicular alpha alumina |
-
2017
- 2017-01-03 CN CN201710000642.5A patent/CN106830029B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4562059A (en) * | 1984-06-08 | 1985-12-31 | Chiyoda Chemical Engineering & Construction Co., Ltd. | Method of preparing alumina |
| JPH07126011A (en) * | 1993-10-26 | 1995-05-16 | Showa Denko Kk | Method for crystallizing columnar aluminum hydroxide |
| CN101391792A (en) * | 2008-11-11 | 2009-03-25 | 中国铝业股份有限公司 | Method for preparing acicular alpha alumina |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107265487A (en) * | 2017-06-15 | 2017-10-20 | 郑州中绿环保新材料有限公司 | A kind of method that use solid sodium aluminate produces special aluminium hydroxide product |
| CN107265487B (en) * | 2017-06-15 | 2019-04-19 | 郑州中绿环保新材料有限公司 | A method of special aluminium hydroxide product is produced using solid sodium aluminate |
| CN112028095A (en) * | 2020-08-12 | 2020-12-04 | 中铝山东有限公司 | Superfine aluminum hydroxide seed crystal and preparation method thereof, submicron aluminum hydroxide and preparation method and application thereof |
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| CN106830029B (en) | 2018-12-18 |
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