CN110255583A - A method of preparing potassium chloride - Google Patents
A method of preparing potassium chloride Download PDFInfo
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- CN110255583A CN110255583A CN201910588331.4A CN201910588331A CN110255583A CN 110255583 A CN110255583 A CN 110255583A CN 201910588331 A CN201910588331 A CN 201910588331A CN 110255583 A CN110255583 A CN 110255583A
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- 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
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- 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
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Abstract
The invention discloses a kind of methods for preparing potassium chloride, belong to chemical industry of inorganic salt technical field.The present invention is using FBRM to the partial size and grain number distribution progress on-line analysis during low-sodium carnalite crystallisation by cooling preparing potassium chloride, image in monitoring crystallization process is combined with PVM simultaneously, realize the multi-angular analysis in potassium chloride crystallization process, the crystal grain of certain particle size range is prepared with the analysis property of can choose by this monitoring, and this is conducive to the yield and quality that improve product, it is connected using in the technique of carnallite production potassium chloride using two sections of crystallization reactors, it not only ensure that the complete decomposition of the low-sodium carnalite in crystallization processes, and fundamentally reduce the dosage of fresh water in crystallization operation, to reduce the KCE content in overflowing liquid, make to significantly improve using the yield of present invention process production potassium chloride.
Description
Technical field
The present invention relates to chemical industry of inorganic salt technical field more particularly to a kind of methods for preparing potassium chloride.
Background technique
Potassium chloride is both the main component of a kind of important chemical raw material and potash fertilizer.Prior art mostly uses reverse flotation-
Cold crystallization technique produces Potassium Chloride Product, is conceived to finished product quality problems more, opposite to Study on Crystallization Process to be short of, and deposits always
It is low in the rate of recovery, the problems such as product quality is not high, energy consumption is high, and these problems are closely bound up with product granularity.
PrliaeKardum et al. has studied the crystallisation by cooling process of potassium chloride, and discovery stirring rate is affected to crystallization shape,
250r·min-1Under the conditions of have part acicular crystal appearance, revolving speed 350rmin-1More than, it is essentially blocky.Liu Chang et al.[4]
Carnallite is had studied in pure water, KCl solution and MgCl2The growth pattern of KCl crystallization is different when decomposing in solution, it is indicated that water-soluble
The cellular KCl crystallization formed in liquid.Feng Shuo[5]KCl is had studied in KCl-MgCl2-H2Thermodynamics of crystallization and power in O system
It learns, and in 50 DEG C, reactant concentration 0.04molkg-1Under the conditions of obtained superior in quality cube KCl crystal.It is existing
Document has some reports to the dynamic research of carnallite crystalliser pan heat, is concentrated mainly on MgCl in decomposed solution2Content, turns degree of supersaturation
The influence to Metastable zone such as speed, rate of temperature fall, residence time, it is less to the Research Literature of particle diameter distribution, and good partial size point
Cloth is conducive to obtain target particles crystallization, improves target crystalline quality.
Thus how from particle diameter distribution determine the invention of method for preparing potassium chloride a kind of to improve potassium chloride quality and
Yield has key effect.
Summary of the invention
It is an object of the invention to: when in order to solve to prepare crystallisation by cooling during potassium chloride, it cannot control effectively
The particle diameter distribution of potassium chloride crystal grain obtains target crystal grain, and leads to gained potassium chloride quality and the lower problem of yield, and mentions
A kind of method preparing potassium chloride out.
To achieve the goals above, present invention employs following technical solutions:
A method of preparing potassium chloride, it is characterised in that specific preparation step are as follows:
Smart potassium solution is subjected to mechanical stirring with the revolving speed of 200~400r/min, crystallisation by cooling controls crystallisation by cooling rate
For 0.1~0.3k.min-1, until 20~30min after crystallization generation, is centrifuged, then do after precipitated crystal taking-up is washed with fresh water
It is dry to obtain refined potassium chloride of the invention.
The specific preparation step of smart potassium solution are as follows:
(1) fresh water of equivalent is added into primary crystallization reactor and secondary crystallization reactor, then low-sodium carnalite is divided
It is not added in primary crystallization reactor and secondary crystallization reactor, stirring forms slurry, shape in subsequent primary crystallization reactor
At underflow slurry pipeline transport continue decomposition and crystallization into secondary crystallization reactor, thick potassium is decomposed to form in secondary crystallization reactor
Slurry；
(2) after above-mentioned thick potassium slurry being removed bulky grain sodium chloride by Vibration Screen, water is added, smart potassium solution is obtained.
It is as above-mentioned technical proposal to further describe:
Agitating mode of the invention is preferably stirred with two leaf plastic stir paddles in the potassium chloride preparation step.
It is as above-mentioned technical proposal to further describe:
The crystallization generation refers to the node that peak crystallization enters the crystalline growth phase occur.
It is as above-mentioned technical proposal to further describe:
Crystallisation by cooling process FBRM records overall process crystallization grain number and particle diameter distribution, observes crystallization process with PVM
Crystallization after reaction, to determine that peak crystallization occur enters the node of crystalline growth phase and the partial size of crystallisation by cooling process
Distribution.
It is as above-mentioned technical proposal to further describe:
In the essence specific preparation step of potassium solution (1) in primary crystallization reactor and secondary crystallization reactor slurry salt
Mass content is respectively 50~65%, 35~45%.
It is as above-mentioned technical proposal to further describe:
Potassium chloride mass content is greater than in low-sodium carnalite described in the essence specific preparation step of potassium solution (1)
22.5%, sodium chloride mass content is less than 5%.
It is as above-mentioned technical proposal to further describe:
The bulky grain sodium chloride partial size that Vibration Screen removes in the essence specific preparation step of potassium solution (2) is less than 100 mesh.
It is as above-mentioned technical proposal to further describe:
1.4~1.6g/cm of the smart potassium solution density of gained in the essence specific preparation step of potassium solution (2)3。
In conclusion by adopting the above-described technical solution, the beneficial effects of the present invention are:
1, the present invention using FBRM to during low-sodium carnalite crystallisation by cooling preparing potassium chloride partial size and grain number distribution
On-line analysis is carried out, while being combined image in monitoring crystallization process with PVM, is realized polygonal in potassium chloride crystallization process
Degree is analyzed, and prepares the crystal grain of certain particle size range with the analysis property of can choose by this monitoring, and this is conducive to improve production
The yield and quality of product.
2, the present invention compared with the prior art, it is of the present invention using carnallite production potassium chloride technique have with
Lower advantage: the present invention is connected in the technique using carnallite production potassium chloride using two sections of crystallization reactors, is not only guaranteed
In the crystallization processes complete decomposition of low-sodium carnalite, and fundamentally reduce the dosage of fresh water in crystallization operation, from
And the KCE content in overflowing liquid is reduced, make to significantly improve using the yield of present invention process production potassium chloride.
Detailed description of the invention
Fig. 1 is the potassium chloride grain number distribution map that embodiment 1,2,3 generates.
Fig. 2 is the grain size distribution that embodiment 1,2,3 generates.
Fig. 1, Fig. 2 are FBRM record the data obtained figure.
Fig. 3 is the crystal grain picture that embodiment 1,2,3 observes crystallization process using PVM at the end of reaction.
Specific embodiment
The fresh water of equivalent is added into primary crystallization reactor and secondary crystallization reactor, then low-sodium carnalite is added respectively
Enter into primary crystallization reactor and secondary crystallization reactor, stirring forms slurry, wherein primary crystallization reactor and secondary knot
The salt quality content of slurry is respectively 50~65%, 35~45% in brilliant reactor, is formed in subsequent primary crystallization reactor
Underflow slurry pipeline transport continues decomposition and crystallization into secondary crystallization reactor, and thick potassium material is decomposed to form in secondary crystallization reactor
It starches, potassium chloride mass content is greater than 22.5% in the low-sodium carnalite, and sodium chloride mass content is less than 5%；It will be above-mentioned thick
After potassium slurry removes bulky grain sodium chloride by Vibration Screen, water is added, smart potassium solution is obtained, this moment smart potassium solution density 1.4
~1.6g/cm3.Above-mentioned smart potassium solution is subjected to mechanical stirring, crystallisation by cooling, control cooling with the revolving speed of 200~400r/min
Crystalline rate is 0.1~0.3k.min-1, until crystallization generate after 20~30min, after precipitated crystal taking-up is washed with fresh water from
The heart, re-dry obtain refined potassium chloride of the invention, and agitating mode of the invention is preferably stirred with two leaf plastic stir paddles,
The crystallization generation refers to the node that peak crystallization enters the crystalline growth phase occur, and crystallisation by cooling process records overall process with FBRM
Grain number and particle diameter distribution are crystallized, crystallization with PVM observation crystallization process and after reaction, to determine that peak crystallization occur enters knot
The node of crystals growth phase and the particle diameter distribution of crystallisation by cooling process.
Embodiment 1
The fresh water of equivalent is added into primary crystallization reactor and secondary crystallization reactor, then low-sodium carnalite is added respectively
Enter into primary crystallization reactor and secondary crystallization reactor, stirring forms slurry, wherein primary crystallization reactor and secondary knot
The salt quality content of slurry is respectively 60%, 40% in brilliant reactor, the underflow slurry formed in subsequent primary crystallization reactor
It is transported in secondary crystallization reactor and continues decomposition and crystallization, thick potassium slurry is decomposed to form in secondary crystallization reactor, it is described
Potassium chloride mass content is greater than 22.5% in low-sodium carnalite, and sodium chloride mass content is less than 5%；Above-mentioned thick potassium slurry is passed through
After Vibration Screen removes bulky grain sodium chloride, water is added, smart potassium solution is obtained, this moment smart potassium solution density 1.5g/cm3.It will be upper
It states smart potassium solution and mechanical stirring is carried out with the revolving speed of 200r/min with two leaf plastic stir paddles, crystallisation by cooling controls crystallisation by cooling
Rate is 0.2k.min-1, until 25min after crystallization generation, is centrifuged, re-dry obtains after precipitated crystal taking-up is washed with fresh water
Refined potassium chloride of the invention, the crystallization generation refer to the node that peak crystallization enters the crystalline growth phase occur, crystallisation by cooling
Process FBRM records overall process crystallization grain number and particle diameter distribution, crystallization with PVM observation crystallization process and after reaction, with
Determine that peak crystallization occur enters the node of crystalline growth phase and the particle diameter distribution of crystallisation by cooling process.
Embodiment 2
The fresh water of equivalent is added into primary crystallization reactor and secondary crystallization reactor, then low-sodium carnalite is added respectively
Enter into primary crystallization reactor and secondary crystallization reactor, stirring forms slurry, wherein primary crystallization reactor and secondary knot
The salt quality content of slurry is respectively 60%, 50% in brilliant reactor, the underflow slurry formed in subsequent primary crystallization reactor
It is transported in secondary crystallization reactor and continues decomposition and crystallization, thick potassium slurry is decomposed to form in secondary crystallization reactor, it is described
Potassium chloride mass content is greater than 22.5% in low-sodium carnalite, and sodium chloride mass content is less than 5%；Above-mentioned thick potassium slurry is passed through
After Vibration Screen removes bulky grain sodium chloride, water is added, smart potassium solution is obtained, this moment smart potassium solution density 1.5g/cm3.It will be upper
It states smart potassium solution and mechanical stirring is carried out with the revolving speed of 300r/min with two leaf plastic stir paddles, crystallisation by cooling controls crystallisation by cooling
Rate is 0.2k.min-1, until 25min after crystallization generation, is centrifuged, re-dry obtains after precipitated crystal taking-up is washed with fresh water
Refined potassium chloride of the invention, the crystallization generation refer to the node that peak crystallization enters the crystalline growth phase occur, crystallisation by cooling
Process FBRM records overall process crystallization grain number and particle diameter distribution, crystallization with PVM observation crystallization process and after reaction, with
Determine that peak crystallization occur enters the node of crystalline growth phase and the particle diameter distribution of crystallisation by cooling process.
Embodiment 3
The fresh water of equivalent is added into primary crystallization reactor and secondary crystallization reactor, then low-sodium carnalite is added respectively
Enter into primary crystallization reactor and secondary crystallization reactor, stirring forms slurry, wherein primary crystallization reactor and secondary knot
The salt quality content of slurry is respectively 55%, 40% in brilliant reactor, the underflow slurry formed in subsequent primary crystallization reactor
It is transported in secondary crystallization reactor and continues decomposition and crystallization, thick potassium slurry is decomposed to form in secondary crystallization reactor, it is described
Potassium chloride mass content is greater than 22.5% in low-sodium carnalite, and sodium chloride mass content is less than 5%；Above-mentioned thick potassium slurry is passed through
After Vibration Screen removes bulky grain sodium chloride, water is added, smart potassium solution is obtained, this moment smart potassium solution density 1.6g/cm3.It will be upper
It states smart potassium solution and mechanical stirring is carried out with the revolving speed of 400r/min with two leaf plastic stir paddles, crystallisation by cooling controls crystallisation by cooling
Rate is 0.3k.min-1, until 30min after crystallization generation, is centrifuged, re-dry obtains after precipitated crystal taking-up is washed with fresh water
Refined potassium chloride of the invention, the crystallization generation refer to the node that peak crystallization enters the crystalline growth phase occur, crystallisation by cooling
Process FBRM records overall process crystallization grain number and particle diameter distribution, crystallization with PVM observation crystallization process and after reaction, with
Determine that peak crystallization occur enters the node of crystalline growth phase and the particle diameter distribution of crystallisation by cooling process.
Figure of description 1,2,3 according to the present invention is it is found that the present invention utilizes FBRM, PVM to remember during preparing potassium chloride
Overall process is recorded, thus wanted target potassium chloride, and gained can be obtained with the particle size range of potassium chloride obtained by autonomous control
Potassium chloride crystal grain quality is stablized, and yield is higher.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of method for preparing potassium chloride, it is characterised in that specific preparation step are as follows:
Smart potassium solution is subjected to mechanical stirring, crystallisation by cooling with the revolving speed of 200~400r/min, control crystallisation by cooling rate is
0.1~0.3k.min-1, until 20~30min after crystallization generation, is centrifuged, re-dry after precipitated crystal taking-up is washed with fresh water
Obtain refined potassium chloride of the invention.
The specific preparation step of smart potassium solution are as follows:
(1) fresh water of equivalent is added into primary crystallization reactor and secondary crystallization reactor, then low-sodium carnalite is added respectively
Enter into primary crystallization reactor and secondary crystallization reactor, stirring forms slurry, is formed in subsequent primary crystallization reactor
Underflow slurry pipeline transport continues decomposition and crystallization into secondary crystallization reactor, and thick potassium material is decomposed to form in secondary crystallization reactor
Slurry；
(2) after above-mentioned thick potassium slurry being removed bulky grain sodium chloride by Vibration Screen, water is added, smart potassium solution is obtained.
2. a kind of method for preparing potassium chloride according to claim 1, which is characterized in that in the potassium chloride preparation step
Agitating mode of the invention is preferably stirred with two leaf plastic stir paddles.
3. a kind of method for preparing potassium chloride according to claim 1, which is characterized in that the crystallization generation refers to appearance
Peak crystallization enters the node of crystalline growth phase.
4. a kind of method for preparing potassium chloride according to claim 1, which is characterized in that the crystallisation by cooling process is used
FBRM records overall process crystallization grain number and particle diameter distribution, crystallization with PVM observation crystallization process and after reaction, to determine
Existing peak crystallization enters the node of crystalline growth phase and the particle diameter distribution of crystallisation by cooling process.
5. a kind of method for preparing potassium chloride according to claim 1, which is characterized in that the essence potassium solution is specifically prepared
In step (1) in primary crystallization reactor and secondary crystallization reactor the salt quality content of slurry be respectively 50~65%, 35~
45%.
6. a kind of method for preparing potassium chloride according to claim 1, which is characterized in that the essence potassium solution is specifically prepared
Potassium chloride mass content is greater than 22.5% in low-sodium carnalite described in step (1), and sodium chloride mass content is less than 5%.
7. a kind of method for preparing potassium chloride according to claim 1, which is characterized in that the essence potassium solution is specifically prepared
The bulky grain sodium chloride partial size that Vibration Screen removes in step (2) is less than 100 mesh.
8. a kind of method for preparing potassium chloride according to claim 1, which is characterized in that the smart specific preparation step of potassium solution
(2) 1.4~1.6g/cm of the smart potassium solution density of gained in3。
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| CN201910588331.4A CN110255583A (en) | 2019-07-02 | 2019-07-02 | A method of preparing potassium chloride |
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| CN201910588331.4A CN110255583A (en) | 2019-07-02 | 2019-07-02 | A method of preparing potassium chloride |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106178583A (en) * | 2016-09-20 | 2016-12-07 | 武汉科技大学 | The feedback of crystal product granularity during a kind of dilution crystallization |
| CN108862328A (en) * | 2018-06-29 | 2018-11-23 | 青海盐湖工业股份有限公司 | A kind of technique using carnallite production potassium chloride |
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2019
- 2019-07-02 CN CN201910588331.4A patent/CN110255583A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106178583A (en) * | 2016-09-20 | 2016-12-07 | 武汉科技大学 | The feedback of crystal product granularity during a kind of dilution crystallization |
| CN108862328A (en) * | 2018-06-29 | 2018-11-23 | 青海盐湖工业股份有限公司 | A kind of technique using carnallite production potassium chloride |
Non-Patent Citations (1)
| Title |
|---|
| 王杏等: "黑钛液中七水硫酸亚铁结晶动力学性质", 《化工学报》 * |
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Application publication date: 20190920 |