CN109019636A - A method of food-grade potassium chloride is produced using the salt of tail containing potassium - Google Patents
A method of food-grade potassium chloride is produced using the salt of tail containing potassium Download PDFInfo
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- CN109019636A CN109019636A CN201811252801.1A CN201811252801A CN109019636A CN 109019636 A CN109019636 A CN 109019636A CN 201811252801 A CN201811252801 A CN 201811252801A CN 109019636 A CN109019636 A CN 109019636A
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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
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The present invention provides a kind of method for producing food-grade potassium chloride using the salt of tail containing potassium, comprising: carries out hydrolyzable to the salt of tail containing potassium, and is filtered to the slurry after decomposition, obtains bittern containing potassium；The bittern containing potassium is carried out to shine obtained sylvite, and heat of solution is carried out to the sylvite, obtains lysate；Supernatant is obtained after carrying out enrichment to the lysate and addition filter aid obtains refined potassium chloride solution after being cleaned containing the underflow of sodium chloride particle, and into the supernatant；To obtaining food-grade potassium chloride after the refined potassium chloride solution crystallisation by cooling, separation of solid and liquid.Method provided by the invention has many advantages, such as to economize on resources, reduces production cost, is easy to operate, is with a wide range of applications.
Description
Technical field
The invention belongs to inorganic chemicals industry food processing fields, produce food using the salt of tail containing potassium more particularly, to a kind of
The method of grade potassium chloride.
Background technique
Food-grade potassium chloride is widely used in the tune of agricultural product, aquatic products, livestock products, fermentation product, flavouring, instant food
Taste agent etc., market development potential is big.Food-grade potassium chloride production at present not yet forms scale in west area, there is biggish market
Space.The diversification of sylvite product, high-valued exploitation can promote the sustainable healthy benign development of salt lake potassium industry, extend salt lake
The industrial chain of potassium industry lead salt lake resources not only in industry, agriculture field development, can also by improving added value to food
Domain development.
The technology of preparing of existing food-grade potassium chloride is using industrial potassium chloride as raw material, by thermosol-cold crystallization process
Middle coupling chemistry impurity removal method is added lye and removes calcium ion, magnesium ion, then by way of aoxidizing or adsorbing or be heated at high temperature
Floating agent is removed, finally realizes that deep impurity-removing, complex process, production cost are higher by multi-step subtractive process.
Industrial potassium chloride can generate a large amount of waste, that is, the salt of tail containing potassium in process of production, wherein potassium chloride
Content is squeezed into designated place by tail salt pump and is stored up about between 2%-15%, chloride containing potassium portion in the tail salt after stockpiling
Divide and waste is caused not to be available.Such as the salt of tail containing potassium that Qinghai Salt Lake Industry Co., Ltd. discharges every year just has more than 600 ten thousand
Ton, wherein KCE content is also most conservative number in terms of 4% in tail salt, and the potassium chloride lost in tail salt every year just has 24
As many as ten thousand tons, recycled under potassium resource status increasingly in short supply this part potassium resource be walk salt lake resources comprehensive utilization and it is sustainable
The only way of exploitation.
Summary of the invention
The technical problem to be solved in the present invention is that a kind of method for producing food-grade potassium chloride using the salt of tail containing potassium is provided,
To solve the problems, such as in existing food-grade potassium chloride technology of preparing there are complex process and production cost are higher, while recycling benefit
With the potassium chloride in the salt of tail containing potassium, solves the problems, such as that potassium resource wastes, promote sustainable development.
The invention provides the following technical scheme: a kind of method for producing food-grade potassium chloride using the salt of tail containing potassium, comprising: right
The salt of tail containing potassium carries out hydrolyzable, and is filtered to the slurry after decomposition, obtains bittern containing potassium；To the bittern containing potassium
It carries out shining obtained sylvite, and heat of solution is carried out to the sylvite, obtain lysate；It is obtained after carrying out enrichment to the lysate
To supernatant and containing the underflow of sodium chloride particle, and it is added after filter aid is cleaned into the supernatant and obtains purification chlorine
Change potassium solution；To obtaining food-grade potassium chloride after the refined potassium chloride solution crystallisation by cooling, separation of solid and liquid.
According to embodiment of the present invention, wherein to the salt of tail containing potassium carry out hydrolyzable, and to decomposition after
Slurry is filtered, and obtains bittern containing potassium, comprising: is transported to the salt of tail containing potassium and is decomposed in tank, adds water and stirs, make tail containing potassium
All dissolution enters liquid phase for potassium chloride and magnesium chloride in salt, and sodium chloride only enters liquid phase on a small quantity, remaining is with solid phase form
In the presence of slurry after being decomposed；Concentrator is squeezed into the slurry after the decomposition and carries out enrichment, is removed by concentrator overflow
The sodium chloride foam on surface, thickener underflow are squeezed into filter and are separated by solid-liquid separation, and bittern containing potassium is obtained.
According to embodiment of the present invention, further comprise: filter being squeezed into thickener underflow and carries out solid-liquid point
Solid phase from rear generation is eluted, and industrial chlorinations sodium is obtained.
According to embodiment of the present invention, wherein the bittern containing potassium is carried out to shine obtained sylvite, comprising: logical
Natural evaporation is crossed, sylvite is precipitated after evaporating fresh water using Phase Diagram for Aqueous Salt Solutions principle, and the old halogen after solarization sylvite processed is arranged
Enter salt pan and further recycles magnesium and lithium in old halogen.
According to embodiment of the present invention, wherein to the sylvite carry out heat of solution temperature control 60 DEG C-
Between 100 DEG C.
According to embodiment of the present invention, further comprise: solid-liquid point is carried out to the underflow containing sodium chloride particle
Solid phase from rear generation is eluted, and industrial chlorinations sodium is obtained, and the liquid phase generated after separation of solid and liquid returns to heat of solution process and repeats
It utilizes.
According to embodiment of the present invention, wherein be added after filter aid is cleaned and obtain into the supernatant
Refined potassium chloride solution, comprising: filter aid is added into the supernatant, keeps calcium ion in the supernatant and magnesium ion clear
Drop, while the organic matter in the supernatant is adsorbed, the method for recycling separation of solid and liquid removes sediment, to realize removal of impurities
Purpose obtains refined potassium chloride solution.
According to embodiment of the present invention, further comprise: the sediment is washed, by filter aid and miscellaneous
Matter separates, and obtains the qualified filter aid of washing.
According to embodiment of the present invention, further comprise: by the refined potassium chloride solution crystallisation by cooling, solid-liquid
Liquid phase obtained after separation returns to the recycling of heat of solution process.
A kind of method for utilizing the salt of tail containing potassium to produce food-grade potassium chloride provided by the invention has the advantages that containing potassium
Tail salt is raw material, recycles the potassium chloride in the salt of tail containing potassium, and potassium resource is promoted to recycle；Technical grade chlorination is produced in thermosol
By increasing removal of impurities process in the technique of potassium, food-grade potassium chloride is obtained, the drying and dissolution of industrial potassium chloride production are reduced
Process shortens process flow, reduces production cost；By the way that filter aid is added into supernatant, make calcium ion in supernatant and
The clear drop of magnesium ion, while the organic matter in supernatant is adsorbed, realize the purpose of removal of impurities, compared with prior art, impurity removal process letter
It is single, easy to operate, therefore, it is provided by the invention it is a kind of using the salt of tail containing potassium produce food-grade potassium chloride method have save money
Source, reduce production cost, it is easy to operate the advantages that, be with a wide range of applications.
Detailed description of the invention
Fig. 1 is a kind of process flow chart that food-grade potassium chloride is produced using the salt of tail containing potassium provided by the invention.
Fig. 2 is the more optimized process flow provided by the invention that food-grade potassium chloride method is produced using the salt of tail containing potassium
Figure.
Specific embodiment
The preferred embodiments of the present invention will be described in detail with reference to the accompanying drawing, and reference label refers to the group in the present invention
Part, technology, realizing under appropriate circumstances so as to advantages and features of the invention can be easier to be understood.Following description is pair
The materialization of the claims in the present invention, and other specific implementations not clearly stated relevant to claim also belong to power
The range that benefit requires.
Fig. 1 shows a kind of process flow chart that food-grade potassium chloride is produced using the salt of tail containing potassium provided by the invention.
As shown in Figure 1, the present invention provides a kind of method for producing food-grade potassium chloride using the salt of tail containing potassium, comprising: to institute
It states the salt of tail containing potassium and carries out hydrolyzable, and the slurry after decomposition is filtered, obtain bittern containing potassium；To the bittern containing potassium into
Row, which shines, is made sylvite, and carries out heat of solution to the sylvite, obtains lysate；It is obtained after carrying out enrichment to the lysate
Supernatant and underflow containing sodium chloride particle, and be added after filter aid is cleaned into the supernatant and obtain purification chlorination
Potassium solution；To obtaining food-grade potassium chloride after the refined potassium chloride solution crystallisation by cooling, separation of solid and liquid.
The above salt of tail containing potassium exists in the form of ore pulp, including tailing containing potassium and tail washings, main component are shown in Table
1:
Table 1: the salt component analytical table of tail containing potassium
In addition, in the salt of tail containing potassium also containing a small amount of calcium sulfate and it is some left in industrial potassium chloride production process it is floating
Select the organic impurities such as medicament organic amine.
Fig. 2 shows the more optimized technique streams provided by the invention that food-grade potassium chloride method is produced using the salt of tail containing potassium
Cheng Tu.
As shown in Fig. 2, method provided by the invention, wherein to the salt of tail containing potassium carry out hydrolyzable, and to decomposition after
Slurry be filtered, obtain bittern containing potassium, comprising: the salt of tail containing potassium is transported to and is decomposed in tank, is added water and stirred, is made containing potassium
All dissolution enters liquid phase for potassium chloride and magnesium chloride in tail salt, and sodium chloride only enters liquid phase on a small quantity, remaining is with solid phase shape
Formula exists, the slurry after being decomposed；Concentrator is squeezed into the slurry after the decomposition and carries out enrichment, is removed by concentrator overflow
The sodium chloride foam on surface is removed, thickener underflow is squeezed into filter and is separated by solid-liquid separation, and bittern containing potassium is obtained.
Three kinds of potassium chloride, sodium chloride and magnesium chloride mono-salts are shown in Table 2 with the solubility that different temperatures changes in water:
The solubility of 2: three kinds of mono-salts of table in water
It is emphasized that three kinds of substances, in same liquid phase, since common-ion effect exists, solubility be will receive together
The influence of ionic effect and have different degrees of variation.Therefore the method for using hydrolyzable first in the present invention, according to chlorine
Change the solubility of potassium in water, suitable water be added, dissolves potassium chloride and magnesium chloride in the salt of tail containing potassium all and enter liquid phase,
And sodium chloride only enters liquid phase on a small quantity, remaining exists with solid phase form, therefore the method refiltered by hydrolyzable can be with
Remove most of sodium chloride in the salt of tail containing potassium.Show that the variation of the solubility with temperature of sodium chloride is smaller from table 2 simultaneously, because
This method that can use heat of solution removes remaining sodium chloride as impurity.
Method provided by the invention further comprises: squeezing into after filter is separated by solid-liquid separation thickener underflow and generates
Solid phase eluted, obtain industrial chlorinations sodium.
Solid phase among the above is undissolved sodium chloride, and potassium chloride and magnesium chloride for being adhered to above by elution removal etc. are molten
Raw material after the substance of liquid phase, into stockyard, as production soda ash.The mother liquor generated after elution is done back to decomposition process
Solvent uses.
Method provided by the invention, wherein the bittern containing potassium is carried out to shine obtained sylvite, comprising: pass through natural steaming
Sylvite is precipitated after evaporating fresh water using Phase Diagram for Aqueous Salt Solutions principle in hair, and will shine the old halogen after sylvite processed be discharged into salt pan into
One step recycles magnesium and lithium in old halogen, accomplishes the maximization of the utilization of resources and high-valued.
Method provided by the invention, wherein to the sylvite carry out heat of solution temperature control 60 DEG C -100 DEG C it
Between.
Concrete operations are that sylvite is delivered to heat of solution tank to dissolve, and are changed using the solubility with temperature of sodium chloride
Lesser principle, with hot water dissolving's sylvite, temperature is controlled between 60 DEG C -100 DEG C, and potassium chloride and magnesium chloride therein are with temperature
The raising changes in solubility of degree is larger, and all dissolution enters liquid phase, and sodium chloride changes due to solubility with temperature less with solid phase
Form exist, be separated by solid-liquid separation at high temperature, so that it may separate solid-phase chlorination sodium with magnesium chloride and potassium chloride.
Method provided by the invention further comprises: carrying out being separated by solid-liquid separation solid-liquid point to the underflow containing sodium chloride particle
Solid phase from rear generation is eluted, and industrial chlorinations sodium is obtained, and the liquid phase generated after separation of solid and liquid returns to heat of solution process and repeats
It utilizes.
It, need to be first by dissolution due to the lower requirement that separation of solid and liquid is not achieved of lysate concentration after heat of solution in the present invention
Liquid squeezes into concentrator and carries out enrichment, while concentrator takes Insulation to prevent cooling potassium chloride that loss is precipitated in concentrator,
The supernatant of concentrator overflow enters next removal of impurities process, and the underflow that concentrator contains sodium chloride particle carries out solid-liquid at high temperature
Separation, obtained solid phase obtain industrial chlorinations sodium after being eluted, go to stockyard to make the original material of production soda ash, produce after separation of solid and liquid
Raw liquid phase returns to heat of solution process, carries out heat of solution to sylvite again, while the mother liquor generated after eluting also returns to thermosol
Process is solved, so not only can be to liquid phase and disposing mother liquor using reduction outlet, but also waste heat is made full use of, reduce thermal losses.
Method provided by the invention, wherein be added after filter aid is cleaned into the supernatant and obtain purification chlorination
Potassium solution, comprising: filter aid is added into the supernatant, makes calcium ion and the clear drop of magnesium ion in the supernatant, simultaneously
The organic matter in the supernatant is adsorbed, the method for recycling separation of solid and liquid removes sediment and obtains to realize the purpose of removal of impurities
To refined potassium chloride solution.
Removal of impurities in the present invention is after heat of solution removes sodium chloride, this is added while entering surge tank in high temperature supernatant
Speciality filter aid in invention, filter aid not only has the function of clear drop calcium ions and magnesium ions, while can adsorb organic matter, thus
The absorption of calcium ions and magnesium ions clear drop and organic matter may be implemented, then removing sediment using the method for separation of solid and liquid can remove
The organic matters such as remaining calcium ions and magnesium ions and organic amine (floating agent), realize the purpose of removal of impurities in clear liquid.The essence obtained after removal of impurities
Klorvess Liquid processed can meet food-grade potassium chloride requirement index through drying by the solid phase after crystallisation by cooling, separation of solid and liquid.
Method provided by the invention further comprises: the sediment washed, filter aid and impurity are separated,
The qualified filter aid of washing is obtained, realizes that filter aid is recycled, reduces the purpose of cost.
Method provided by the invention further comprises: will obtain after the refined potassium chloride solution crystallisation by cooling, separation of solid and liquid
The liquid phase arrived returns to the recycling of heat of solution process.
Still contain many potassium chloride in the liquid phase obtained after above-mentioned separation of solid and liquid, heat of solution process is returned to, again to potassium stone
Salt carries out heat of solution, not only recycles to liquid phase, while improving the rate of recovery of potassium chloride again.
The requirement index of food-grade potassium chloride is shown in Table 3:
Table 3: the indices of food-grade potassium chloride
Food-grade potassium chloride obtained in the present invention be fully achieved the index in above table 3, especially the total content of magnesium and calcium and
The amount of organic matter reaches standard or more, and wherein KCE content reaches 99.3% or more and is higher than standard, and sodium ions content is less than
0.4% hereinafter, organic matter≤3mg/kg.
A kind of method for utilizing the salt of tail containing potassium to produce food-grade potassium chloride provided by the invention has the advantages that containing potassium
Tail salt is raw material, recycles the potassium chloride in the salt of tail containing potassium, and potassium resource is promoted to recycle；Technical grade chlorination is produced in thermosol
By increasing removal of impurities process in the technique of potassium, food-grade potassium chloride is obtained, the drying and dissolution of industrial potassium chloride production are reduced
Process shortens process flow, reduces production cost；By the way that filter aid is added into supernatant, make calcium ion in supernatant and
The clear drop of magnesium ion, while the organic matter in supernatant is adsorbed, realize the purpose of removal of impurities, compared with prior art, impurity removal process letter
It is single, easy to operate, therefore, it is provided by the invention it is a kind of using the salt of tail containing potassium produce food-grade potassium chloride method have save money
Source, reduce production cost, it is easy to operate the advantages that, be with a wide range of applications.
It should be noted that the above-mentioned embodiments illustrate rather than limit the invention, and this
Field technical staff can be designed alternative embodiment without departing from the scope of the appended claims.In claim
In, any reference symbol between parentheses should not be configured to limitations on claims.
Claims (9)
1. a kind of method for producing food-grade potassium chloride using the salt of tail containing potassium, including:
Hydrolyzable is carried out to the salt of tail containing potassium, and the slurry after decomposition is filtered, obtains bittern containing potassium；
The bittern containing potassium is carried out to shine obtained sylvite, and heat of solution is carried out to the sylvite, obtains lysate；
Supernatant is obtained after carrying out enrichment to the lysate and is added containing the underflow of sodium chloride particle, and into the supernatant
Enter and obtains refined potassium chloride solution after filter aid is cleaned；
To obtaining food-grade potassium chloride after the refined potassium chloride solution crystallisation by cooling, separation of solid and liquid.
2. according to the method described in claim 1, wherein, carrying out hydrolyzable to the salt of tail containing potassium, and to the material after decomposition
Slurry is filtered, and obtains bittern containing potassium, comprising:
The salt of tail containing potassium is transported to and is decomposed in tank, is added water and stirred, keeps potassium chloride in the salt of tail containing potassium and magnesium chloride all molten
Solution enters liquid phase, and sodium chloride only enters liquid phase on a small quantity, remaining exists with solid phase form, the slurry after being decomposed；
Concentrator is squeezed into the slurry after the decomposition and carries out enrichment, the sodium chloride foam on surface is removed by concentrator overflow,
Thickener underflow is squeezed into filter and is separated by solid-liquid separation, and bittern containing potassium is obtained.
3. according to the method described in claim 2, further comprising: squeezing into after filter is separated by solid-liquid separation thickener underflow
The solid phase of generation is eluted, and industrial chlorinations sodium is obtained.
4. according to the method described in claim 1, wherein, carrying out shining obtained sylvite to the bittern containing potassium, comprising:
By natural evaporation, sylvite is precipitated after evaporating fresh water using Phase Diagram for Aqueous Salt Solutions principle, and after sylvite processed being shone
Old halogen is discharged into salt pan and further recycles magnesium and lithium in old halogen.
5. according to the method described in claim 1, wherein, the temperature for carrying out heat of solution to the sylvite is controlled at 60 DEG C -100
Between DEG C.
6. according to the method described in claim 1, further comprising: after being separated by solid-liquid separation to the underflow containing sodium chloride particle
The solid phase of generation is eluted, and industrial chlorinations sodium is obtained, and the liquid phase generated after separation of solid and liquid returns to the recycling of heat of solution process.
7. according to the method described in claim 1, wherein, being added after filter aid is cleaned and being refined into the supernatant
Klorvess Liquid, comprising:
Filter aid is added into the supernatant, makes calcium ion and the clear drop of magnesium ion in the supernatant, while described in absorption
Organic matter in supernatant, the method for recycling separation of solid and liquid removes sediment, to realize the purpose of removal of impurities, obtains purification chlorine
Change potassium solution.
8. according to the method described in claim 7, further comprising: being washed to the sediment, by filter aid and impurity
It separates, obtains the qualified filter aid of washing.
9. according to the method described in claim 1, further comprising: by the refined potassium chloride solution crystallisation by cooling, solid-liquid point
The liquid phase obtained from after returns to the recycling of heat of solution process.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109721079A (en) * | 2019-03-08 | 2019-05-07 | 青海盐湖工业股份有限公司 | A kind of KCl production system and production method |
| CN110590412A (en) * | 2019-10-17 | 2019-12-20 | 青海盐湖工业股份有限公司 | Method for recovering water bath dedusting wastewater in potash fertilizer production |
| CN112441602A (en) * | 2019-08-28 | 2021-03-05 | 中蓝连海设计研究院有限公司 | Salt pan for recovering potassium salt at low cost and method for recovering potassium salt by adopting salt pan |
| CN114408944A (en) * | 2022-01-28 | 2022-04-29 | 中国科学院青海盐湖研究所 | Method for preparing potassium chloride from potassium-containing solid waste |
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| CN102491373A (en) * | 2011-12-22 | 2012-06-13 | 化工部长沙设计研究院 | Method for producing potassium chloride, sodium chloride and magnesium sheet from bittern extracted from carnallite mine |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102491373A (en) * | 2011-12-22 | 2012-06-13 | 化工部长沙设计研究院 | Method for producing potassium chloride, sodium chloride and magnesium sheet from bittern extracted from carnallite mine |
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| 国土资源部矿产资源储量司编著: "含钾尾矿溶解转化热溶结晶法生产氯化钾技术", 《中国矿产资源全面节约和高效利用先进技术实践》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109721079A (en) * | 2019-03-08 | 2019-05-07 | 青海盐湖工业股份有限公司 | A kind of KCl production system and production method |
| CN112441602A (en) * | 2019-08-28 | 2021-03-05 | 中蓝连海设计研究院有限公司 | Salt pan for recovering potassium salt at low cost and method for recovering potassium salt by adopting salt pan |
| CN110590412A (en) * | 2019-10-17 | 2019-12-20 | 青海盐湖工业股份有限公司 | Method for recovering water bath dedusting wastewater in potash fertilizer production |
| CN114408944A (en) * | 2022-01-28 | 2022-04-29 | 中国科学院青海盐湖研究所 | Method for preparing potassium chloride from potassium-containing solid waste |
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