CN107376399A - A kind of method for crystallising of sodium vanadate crystal system and sodium vanadate - Google Patents
A kind of method for crystallising of sodium vanadate crystal system and sodium vanadate Download PDFInfo
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- CN107376399A CN107376399A CN201710708004.9A CN201710708004A CN107376399A CN 107376399 A CN107376399 A CN 107376399A CN 201710708004 A CN201710708004 A CN 201710708004A CN 107376399 A CN107376399 A CN 107376399A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0004—Crystallisation cooling by heat exchange
- B01D9/0013—Crystallisation cooling by heat exchange by indirect heat exchange
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0063—Control or regulation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
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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
- C01P2002/60—Compounds characterised by their crystallite size
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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
- C01P2006/82—Compositional purity water content
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Abstract
The present invention relates to a kind of sodium vanadate crystal system and the method for crystallising of sodium vanadate, the system includes surge tank, heat exchanger, crystallizer, thickener, magma storage tank, filter press and the mother liquor tank set gradually, and the mother liquor tank is connected with thickener supernatant liquid outlet.The sodium vanadate solution being stored in surge tank is delivered in heat exchanger by the present invention, it is delivered to after cooling in crystallizer and carries out crystallization precipitation, the magma of crystalliser feet is delivered to enrichment in thickener, supernatant is stored into mother liquor tank after enrichment, enrichment magma is transported in magma storage tank, then by the isolated vanadic acid sodium crystal of filter press and separating liquid, while gained separating liquid is stored into mother liquor tank.The present invention can effectively control the granularity and moisture of vanadic acid sodium crystal, solve the problems, such as the putty of sodium vanadate crystallization, improve the efficiency of crystal system, realize under the conditions of high alkalinity to the cerium sulphate crystal of sodium vanadate solution, ensure crystal system stabilization, Effec-tive Function, have a good application prospect.
Description
Technical field
The present invention relates to vanadium chemical field, and in particular to a kind of method for crystallising of sodium vanadate crystal system and sodium vanadate.
Background technology
At present, domestic and international vanadium chemical field mostly carries out vanadium extraction using traditional pyrogenic process vanadium slag sodium roasting technique, substantially
Principle is with Na2CO3For additive, the vanadium of lower valency is converted into by water-soluble pentavalent by high temperature sodium roasting (750-850 DEG C)
The sodium salt of vanadium, then to the direct water logging of sodium roasting product, obtain the leaching liquid containing sodium metavanadate, then add ammonium salt and more vanadium are made
Sour ammonium precipitation, the oxide product of vanadium is obtained after reduction roasting.But this method is serious there is carrying capacity of environment, extraction efficiency
Low problem, the demand of current industrial metaplasia production has been not suitable with it.
Wet method vanadium extraction is a kind of extraction vanadium method of cleaning, has the characteristics that environmental protection, efficient, energy consumption is small.This method uses
NaOH solution carries out vanadium extraction, and the solution containing sodium vanadate is obtained by wet process.For example, one is disclosed in CN102531056A
The method of kind vanadium slag pressure leaching clean manufacturing sodium vanadate sodium chromate, this method mixes vanadium slag with NaOH solution, then in oxygen
Pressurization carries out oxidation reaction in the property changed atmosphere, and after gained Solid-liquid mixture is starched into separation of solid and liquid, vanadium is obtained after cleaning, crystallizing
Sour sodium crystal.A kind of method that vanadium is reclaimed by tailings in vanadium extraction is disclosed in CN102251119B, this method includes：By tailings in vanadium extraction
It is added in reactor and is decomposed with water and NaOH, then obtained reaction paste is diluted with water or low-concentration alkali liquor and mixed
Close slurry；Mixed slurry is filtered at 80-130 DEG C, obtains the aqueous solution containing sodium hydroxide, sodium vanadate and sodium metasilicate, desiliconization
Natural cold crystallization obtains vanadate after processing.
Although the above method solves the problems, such as the presence in the preparation process of sodium vanadate, but to the biography of sodium vanadate crystallization
System method equally exists great number of issues, is mainly reflected in：(1) crystallization rate is fast, and sodium vanadate separates out rapidly after cooling, easily blocks knot
Brilliant device or pipeline；(2) crystal grain is uncontrollable, causes sodium vanadate magma filtration difficulty；(3) crystal is in needle-like, during filtering
Easily block filter cloth so that system is unable to continuous and steady operation.Evaporative crystallization technique about pure salt has many case histories, but greatly
It is unsuitable for the crystallization of sodium vanadate under high-alkali system condition.The domestic crystallization to sodium vanadate under high alkali systems at present is not also a set of
Ripe system, so, it is badly in need of developing a set of sodium vanadate crystal system to solve the above problems.
The content of the invention
In view of problems of the prior art, the invention provides a kind of sodium vanadate crystal system and sodium vanadate crystallization side
Method, the system are applied to the crystallization of sodium vanadate under high alkalinity system, can realize under the conditions of high alkalinity to the efficient knot of sodium vanadate
Crystalline substance, the granularity and moisture of sodium vanadate crystal are effectively controlled, the putty for solving the problems, such as sodium vanadate crystallization, improve crystal system
Efficiency.
To use following technical scheme up to this purpose, the present invention：
In a first aspect, the present invention provides a kind of sodium vanadate crystal system, the system includes：The surge tank that sets gradually,
Heat exchanger, crystallizer, thickener, magma storage tank, filter press and mother liquor tank, the thickener be provided with supernatant liquid outlet with
Mother liquor tank is connected.
Crystallizer used in the present invention is excellent to select continuous crystalizer, is realized by using the mode of clear mother liquor forced circulation
The cooling of crystallization process, makes crystalline solid be sunken to crystalliser feet.
According to the present invention, delivery pump is provided between the surge tank and heat exchanger, sodium vanadate solution of the present invention is being tied
The power of crystallographic system system conveying is realized by delivery pump.
According to the present invention, the heat exchanger is spiral heat exchanger.
According to the present invention, the crystallizer is continuous crystalizer.
According to the present invention, the filter press is wire netting filter press.
Second aspect, the present invention provide a kind of method for crystallising of sodium vanadate, are crystallized using the sodium vanadate described in first aspect
System crystallizes to sodium vanadate.The concrete operations of methods described are：The sodium vanadate solution being stored in surge tank is passed through defeated
Send pump to be delivered in heat exchanger, be delivered to after cooling in crystallizer and carry out crystallization precipitation, magma is obtained in crystalliser feet；Will knot
The magma of brilliant device bottom is delivered to enrichment in thickener, obtains enrichment magma and supernatant, supernatant is stored into mother liquor tank；
Enrichment magma is transported in magma storage tank and stored, then by the isolated vanadic acid sodium crystal of filter press press filtration and separating liquid,
Separating liquid obtained by press filtration is stored into mother liquor tank.
Sodium vanadate solution of the present invention is to contain vanadium through what solid-liquor separation obtained after vanadium raw materials extract under high alkali systems
Solution, the sodium vanadate solution are any one in sodium vanadate solution, sodium metavanadate solution or sodium pyrovanadate solution.
According to the present invention, the temperature of sodium vanadate solution is 50-65 DEG C after heat exchanger cools, such as can be 50 DEG C,
51 DEG C, 52 DEG C, 53 DEG C, 54 DEG C, 55 DEG C, 56 DEG C, 57 DEG C, 58 DEG C, 59 DEG C, 60 DEG C, 61 DEG C, 62 DEG C, 63 DEG C, 64 DEG C or 65 DEG C,
And the specific point value between above-mentioned numerical value, as space is limited and for concise consideration, the present invention no longer exclusive list.
According to the present invention, the temperature that the crystallization separates out is 40-45 DEG C, for example, can be 40 DEG C, 41 DEG C, 42 DEG C, 43 DEG C,
Specific point value between 44 DEG C or 45 DEG C, and above-mentioned numerical value, as space is limited and for concise consideration, no longer limit of the invention
Enumerate.
The present invention is to control grain >=1mm of the crystal grain of precipitation by controlling rate of temperature fall when crystallizing and separating out.Institute
It is 5-10 DEG C/h to state rate of temperature fall
Crystallizer used in the present invention is excellent to select continuous crystalizer, is realized by using the mode of clear mother liquor forced circulation
The cooling of crystallization process, makes crystalline solid be sunken to crystalliser feet.
According to the present invention, solid content is 10-50wt% in the enrichment magma, for example, can be 10wt%, 15wt%,
Specific point value between 20wt%, 25wt%, 30wt%, 35wt%, 40wt%, 45wt% or 50wt%, and above-mentioned numerical value,
As space is limited and for concise consideration, the present invention no longer exclusive list.
Solid content of the present invention refers to the mass fraction of solid in magma.
As preferable technical scheme, the method for crystallising of sodium vanadate of the present invention can be：It will be stored in surge tank
Sodium vanadate solution be delivered to by delivery pump in heat exchanger, be delivered to after being cooled to 50-65 DEG C in crystallizer, be cooled to 40-
45 DEG C carry out crystallization precipitation, and it is 5-10 DEG C/h that rate of temperature fall is controlled in crystallization process, make the particle diameter of the crystal grain of precipitation >=
1mm, magma is obtained in crystalliser feet；The magma of crystalliser feet is delivered to enrichment in thickener, obtain enrichment magma and
Supernatant, solid content is 10-50% in enrichment magma, and supernatant is stored into mother liquor tank；Enrichment magma is transported to magma
In storage tank, then by the isolated vanadic acid sodium crystal of filter press press filtration and separating liquid, separating liquid obtained by press filtration is stored to mother
In flow container.
Compared with prior art, the present invention at least has the advantages that：
The present invention sets heat exchanger before crystallizer, and the crystallization rate of sodium vanadate is reduced by way of substep cools；
Meanwhile the cooling of crystallization process is realized by the way of clear mother liquor forced circulation, pass through the crystalline substance for controlling rate of temperature fall to separate out
Particle diameter >=1mm of body particle, the granularity and moisture of vanadic acid sodium crystal are effectively controlled, the putty for solving the problems, such as sodium vanadate crystallization,
Substantially increase the efficiency of crystal system.The present invention is realized to the cerium sulphate crystal of sodium vanadate solution under the conditions of high alkalinity, can
Ensure crystal system stabilization, Effec-tive Function, have a good application prospect.
Brief description of the drawings
Fig. 1 is for the structural representation of sodium vanadate crystal system provided by the invention.
In figure：1- surge tanks, 2- heat exchangers, 3- crystallizers, 4- thickeners, 5- magma storage tanks, 6- filter presses, 7- mother liquors
Tank.
The present invention is described in more detail below.But following examples is only the simple example of the present invention, not generation
Table or limitation the scope of the present invention, protection scope of the present invention are defined by claims.
Embodiment
Further illustrate technical scheme below in conjunction with the accompanying drawings and by embodiment.
The present invention provides a kind of sodium vanadate crystal system in specific embodiment part, as shown in figure 1, the system bag
Include：Surge tank 1, heat exchanger 2, crystallizer 3, thickener 4, magma storage tank 5, filter press 6 and the mother liquor tank 7 set gradually, institute
Mother liquor tank 7 is stated with thickener 4 to be connected.
Preferably, it is provided with delivery pump between the surge tank 1 and heat exchanger 2；The heat exchanger 2 exchanges heat for spiral plate type
Device；The crystallizer 3 is continuous crystalizer；The filter press is wire netting filter press.
The present invention additionally provides a kind of method for crystallising of sodium vanadate in specific embodiment part, and this method utilizes above-mentioned
Sodium vanadate crystal system crystallizes to sodium vanadate.
The concrete operations of methods described are：The sodium vanadate solution being stored in surge tank 1 is delivered to by delivery pump and changed
In hot device 2, it is delivered to after cooling in crystallizer 3 and carries out crystallization precipitation, magma is obtained in crystalliser feet；By crystalliser feet
Magma is delivered to enrichment in thickener 4, obtains enrichment magma and supernatant；Supernatant is stored into mother liquor tank 7, enrichment is brilliant
Slurry is transported in magma storage tank 5, then by the isolated vanadic acid sodium crystal of the press filtration of filter press 6 and separating liquid, by obtained by press filtration
Separating liquid is stored into mother liquor tank 7.
For the present invention is better described, technical scheme is readily appreciated, of the invention is typical but non-limiting
Embodiment is as follows：
Embodiment 1
A kind of sodium vanadate crystal system, including：Surge tank 1, heat exchanger 2, crystallizer 3, thickener 4, the crystalline substance set gradually
Slurry storage tank 5, filter press 6 and mother liquor tank 7, the mother liquor tank 7 are connected with thickener 4.
Delivery pump is provided between the surge tank 1 and heat exchanger 2；The heat exchanger 2 is spiral heat exchanger；The knot
Brilliant device 3 is continuous crystalizer；The filter press is wire netting filter press.
Sodium vanadate is crystallized using above-mentioned crystal system：
Be stored in surge tank 1 80 DEG C of sodium vanadate solution are delivered in heat exchanger 2 by delivery pump, heat exchanger 2
For spiral-plate heat exchanger, coolant media selects softened water, sodium vanadate solution is cooled to after 56 DEG C and is delivered to continuous crystalizer 3
In；The cooling method circulated using supernatant, it is 10 DEG C/h to control rate of temperature fall, and solution is cooled into 45 DEG C carries out crystallization analysis
Go out, magma is obtained in crystalliser feet, after the blanking of crystallized device bottom, magma enters enrichment in thickener 4, obtains enrichment magma
And supernatant, solid content is 45wt% in enrichment magma, and gained supernatant is stored into mother liquor tank 7；Enrichment magma store to
After in magma storage tank 5, it is delivered to filter press 6 and carries out press filtration separation, obtain vanadic acid sodium crystal and separating liquid, the particle diameter of gained crystal
Stored more than 1mm, moisture content 25wt%, while by separating liquid obtained by press filtration into mother liquor tank 7.
Embodiment 2
The present embodiment is crystallized using the crystal system provided in embodiment 1 to sodium vanadate：
Be stored in surge tank 1 85 DEG C of sodium metavanadate solution are delivered in heat exchanger 2 by delivery pump, heat exchanger 2
For spiral-plate heat exchanger, coolant media selects softened water, sodium metavanadate solution is cooled to after 60 DEG C and is delivered to continuous crystalizer 3
In；The cooling method circulated using supernatant, it is 5 DEG C/h to control rate of temperature fall, and solution is cooled into 42 DEG C carries out crystallization precipitation,
Obtain magma in crystalliser feet, after the blanking of crystallized device bottom, magma enter thickener 4 in enrichment, obtain enrichment magma and
Supernatant, solid content is 27wt% in enrichment magma, and gained supernatant is stored into mother liquor tank 7；Enrichment magma is stored to crystalline substance
After starching in storage tank 5, it is delivered to filter press 6 and carries out press filtration separation, obtain vanadic acid sodium crystal and separating liquid, the particle diameter of gained crystal is big
Stored in 1mm, moisture content 18wt%, while by separating liquid obtained by press filtration into mother liquor tank 7.
Applicant states that the present invention illustrates the detailed construction feature of the present invention by above-described embodiment, but the present invention is simultaneously
Above-mentioned detailed construction feature is not limited to, that is, does not mean that the present invention has to rely on above-mentioned detailed construction feature and could implemented.Institute
Belong to those skilled in the art it will be clearly understood that any improvement in the present invention, to the equivalence replacement of part selected by the present invention
And the increase of accessory, selection of concrete mode etc., all fall within protection scope of the present invention and it is open within the scope of.
The preferred embodiment of the present invention described in detail above, still, the present invention are not limited in above-mentioned embodiment
Detail, in the range of the technology design of the present invention, a variety of simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (10)
1. a kind of sodium vanadate crystal system, it is characterised in that the system includes：Surge tank (1), the heat exchanger set gradually
(2), crystallizer (3), thickener (4), magma storage tank (5), filter press (6) and mother liquor tank (7), set on the thickener (4)
There is supernatant liquid outlet to be connected with mother liquor tank (7).
2. sodium vanadate crystal system as claimed in claim 1, it is characterised in that between the surge tank (1) and heat exchanger (2)
Provided with delivery pump.
3. sodium vanadate crystal system as claimed in claim 1, it is characterised in that the heat exchanger (2) exchanges heat for spiral plate type
Device；
Preferably, the crystallizer (3) is continuous crystalizer；
Preferably, the filter press (6) is wire netting filter press.
4. a kind of method for crystallising of sodium vanadate, it is characterised in that utilize the sodium vanadate system of crystallization described in claim any one of 1-3
System crystallizes to sodium vanadate.
5. method as claimed in claim 4, it is characterised in that methods described is：The sodium vanadate that will be stored in surge tank (1)
Solution is delivered in heat exchanger (2) by delivery pump, is delivered to after cooling in crystallizer (3) and is carried out crystallization precipitation, in crystallizer
Bottom obtains magma；The magma of crystalliser feet is delivered to enrichment in thickener (4), obtains enrichment magma and supernatant, will
Supernatant is stored into mother liquor tank (7)；Enrichment magma is transported in magma storage tank (5) and stored, is then pressed by filter press (6)
Isolated vanadic acid sodium crystal and separating liquid are filtered, separating liquid obtained by press filtration is stored into mother liquor tank (7).
6. method as claimed in claim 5, it is characterised in that the sodium vanadate solution is sodium vanadate solution, sodium metavanadate
Any one in solution or sodium pyrovanadate solution.
7. method as claimed in claim 5, it is characterised in that the temperature of sodium vanadate solution is after heat exchanger (2) cooling
50-65℃。
8. method as claimed in claim 5, it is characterised in that the temperature that the crystallization separates out is 40-45 DEG C；
Preferably, it is 5-10 DEG C/h to control rate of temperature fall when the crystallization separates out, and makes particle diameter >=1mm of the crystal grain of precipitation.
9. method as claimed in claim 5, it is characterised in that solid content is 10-50wt% in the enrichment magma.
10. the method as described in claim any one of 4-9, it is characterised in that methods described is：Surge tank (1) will be stored in
In sodium vanadate solution be delivered to by delivery pump in heat exchanger (2), be delivered to after being cooled to 50-65 DEG C in crystallizer (3), drop
Warm to 40-45 DEG C carries out crystallization precipitation, and it is 5-10 DEG C/h that rate of temperature fall is controlled in crystallization process, makes the grain of the crystal grain of precipitation
Footpath >=1mm, magma is obtained in crystalliser feet；The magma of crystalliser feet is delivered to enrichment in thickener (4), obtains enrichment
Magma and supernatant, solid content is 10-50% in enrichment magma；Supernatant is stored into mother liquor tank (7)；Enrichment magma is defeated
It is sent in magma storage tank (5), then by the isolated vanadic acid sodium crystal of filter press (6) press filtration and separating liquid, by obtained by press filtration
Separating liquid is stored into mother liquor tank (7).
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| CN201710708004.9A CN107376399A (en) | 2017-08-17 | 2017-08-17 | A kind of method for crystallising of sodium vanadate crystal system and sodium vanadate |
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| CN201710708004.9A CN107376399A (en) | 2017-08-17 | 2017-08-17 | A kind of method for crystallising of sodium vanadate crystal system and sodium vanadate |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107746078A (en) * | 2017-11-28 | 2018-03-02 | 河钢股份有限公司承德分公司 | A kind of system and method for preparing ammonium metavanadate crystal |
| CN108905265A (en) * | 2018-07-26 | 2018-11-30 | 西安航天华威化工生物工程有限公司 | Sodium vanadate Continuous Cooling Crystallization equipment and its production method |
| CN113184907A (en) * | 2021-05-31 | 2021-07-30 | 河钢承德钒钛新材料有限公司 | Method for purifying sodium chromate |
| CN114275813A (en) * | 2021-12-30 | 2022-04-05 | 中国科学院过程工程研究所 | Method for flash evaporation, cooling and crystallization of sodium vanadate in alkali liquor system |
| CN115072778A (en) * | 2022-07-27 | 2022-09-20 | 西安航天华威化工生物工程有限公司 | Ammonium polyvanadate continuous reaction crystallization process |
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| CN103991997A (en) * | 2014-05-30 | 2014-08-20 | 中国石油集团东北炼化工程有限公司吉林设计院 | Strong brine evaporating and crystallizing system |
| CN203959976U (en) * | 2014-05-30 | 2014-11-26 | 中国石油集团东北炼化工程有限公司吉林设计院 | Strong brine function of mechanical steam recompression evaporation and crystallization system |
| CN105525096A (en) * | 2016-01-04 | 2016-04-27 | 攀钢集团攀枝花钢钒有限公司 | Recycling method of acid ammonium salt precipitating vanadium waste water |
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| CN103991997A (en) * | 2014-05-30 | 2014-08-20 | 中国石油集团东北炼化工程有限公司吉林设计院 | Strong brine evaporating and crystallizing system |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107746078A (en) * | 2017-11-28 | 2018-03-02 | 河钢股份有限公司承德分公司 | A kind of system and method for preparing ammonium metavanadate crystal |
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| CN113184907A (en) * | 2021-05-31 | 2021-07-30 | 河钢承德钒钛新材料有限公司 | Method for purifying sodium chromate |
| CN114275813A (en) * | 2021-12-30 | 2022-04-05 | 中国科学院过程工程研究所 | Method for flash evaporation, cooling and crystallization of sodium vanadate in alkali liquor system |
| CN114275813B (en) * | 2021-12-30 | 2022-09-02 | 中国科学院过程工程研究所 | Method for flash evaporation, cooling and crystallization of sodium vanadate in alkali liquor system |
| CN115072778A (en) * | 2022-07-27 | 2022-09-20 | 西安航天华威化工生物工程有限公司 | Ammonium polyvanadate continuous reaction crystallization process |
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