CN110127726A - A kind of preparation method of fused salt chlorimation potassium - Google Patents
A kind of preparation method of fused salt chlorimation potassium Download PDFInfo
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- CN110127726A CN110127726A CN201910580727.4A CN201910580727A CN110127726A CN 110127726 A CN110127726 A CN 110127726A CN 201910580727 A CN201910580727 A CN 201910580727A CN 110127726 A CN110127726 A CN 110127726A
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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
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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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- 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 relates to fused salt chlorimation potassium extractive technique fields, disclose a kind of preparation method of fused salt chlorimation potassium, the following steps are included: S1, potassium chloride dissolving powder, take 1000 milliliters of cold water, it is heated to 40 DEG C -90 DEG C, potassium chloride powder is added at 40 DEG C -90 DEG C and dissolves by 250-350 grams of potassium chloride powder again, produces the Klorvess Liquid that mass concentration is 25%~35%；S2, production solution A, the resulting concentration of Xiang Suoshu step S1 are that excessive barium chloride solution is added in 25%~35% Klorvess Liquid, precipitate sulfate ion, filter to obtain solution A；S3, production solution B.The preparation method of the fused salt chlorimation potassium, by potassium chloride dissolving powder, production solution A, refilter solution B, make solution C again, finally solution C is evaporated under reduced pressure, decrease temperature crystalline obtains wet potassium chloride, wet potassium chloride high-temperature calcination is purified into obtain fused salt chlorimation potassium again, solves the problem of current China's fused salt chlorimation potassium extractive technique is backward, and potassium chloride of the country for molten salt system relies primarily on import.
Description
Technical field
The present invention relates to potassium chloride purification technique field, specially a kind of preparation method of fused salt chlorimation potassium.
Background technique
Potassium chloride be white crystalline powder or colourless crystallization, it is soluble easily in water, can be used as savory agent, nutritional supplement；In order to
Inhibit people that can make the substitute of part salt to excess salt intake；It is same as salt be used as agricultural production, aquatic products, livestock products, fermentation,
The flavoring agent of the varieties of food items such as seasoning, can, instant food；As a kind of common used material for constituting inorganic fused salt, used extensively
In various inorganic fused salts.
Fused salt is molten mass composed by metal cation and metalloid anion.It is fused salt metallothermic processes or fused salt
Electrolysis method produces valuable and rare metal critical material.If scandium chloride-sodium chloride-potassium chloride fused salt is among metal scandium and scandium
The critical material of alloying technology；Potassium floutaramite-potassium fluoride-potassium chloride fused salt is the key that electrolysis method high-purity tantalum powder material
Material.
More stringent requirements are proposed to potassium chloride purity for fused salt chlorimation potassium, to calcium, magnesium, metal ion and sulfate, carbonic acid
Salt, organic matter, the index requests such as granularity are very harsh, and current domestic potassium chloride is unable to satisfy its requirement, production technology quilt
Western developed country monopolization.Potassium chloride of the country for molten salt system relies primarily on import, expensive, and country will spend every year
A large amount of foreign exchanges.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, it the present invention provides a kind of preparation method of fused salt chlorimation potassium, can successfully extract
Qualified fused salt chlorimation potassium solves the problems, such as that current China's fused salt chlorimation potassium extractive technique falls behind.
(2) technical solution
To realize the above-mentioned fused salt chlorimation potassium purpose for successfully extracting qualification, the invention provides the following technical scheme: a kind of molten
The preparation method of salt potassium chloride, comprising the following steps:
S1, potassium chloride dissolving powder
1000 milliliters of cold water are taken, 40 DEG C -90 DEG C, then 250-350 grams of potassium chloride powder is heated to, potassium chloride powder is added
Enter and dissolved at 40 DEG C -90 DEG C, produces the Klorvess Liquid that mass concentration is 25%~35%.
S2, production solution A
It is that excessive barium chloride solution is added in 25%~35% Klorvess Liquid to the resulting concentration of step S1, makes
Sulfate ion precipitating, filters to obtain solution A.
S3, production solution B
Excessive potassium carbonate and potassium hydroxide solution are added into the step S2 acquired solution A, makes calcium chloride, magnesium chloride and
Chlorination precipitated barium filters to obtain solution B.
S4, production solution C
Excessive hydrochloric acid is added into the step S3 acquired solution B, converts potassium chloride for excessive potassium carbonate, obtains solution
C。
S5, the wet potassium chloride of production
Acquired solution C in the step S4 is evaporated under reduced pressure, decrease temperature crystalline obtains wet potassium chloride.
S6, purification
Wet potassium chloride high-temperature calcination obtained by the step S5 is purified into obtain fused salt chlorimation potassium.
Preferably, potassium chloride described in step S1 is industry or agricultural potassium chloride, when dissolution can using agitating device into
Row stirring, accelerates dissolution.
Preferably, the barium chloride of addition described in the step S2 is excessively 2%-6%.
Preferably, the potassium carbonate and potassium hydroxide of addition described in the step S3 excessive 3%~5%.
Preferably, the food grade hydrochloric acid that the hydrochloric acid of addition described in the step S4 is excessive 2%~5%.
Preferably, being evaporated under reduced pressure in the step S5 refers to vacuum degree in (- 0.080MPa)~(- 0.085MPa), step
Decrease temperature crystalline in S5,1-3 DEG C of cooling rate/min.
Preferably, high-temperature calcination described in the step S1 purifies, and calcination temperature is at 300-600 DEG C, and calcination time is 20
~40min.
Preferably, gained potassium chloride in the step S6, content >=99.8%, calcination loss≤0.05% (500 DEG C,
2hr), calcium≤5ppm, magnesium≤5ppm, sodium≤30ppm, sulfate≤5ppm, carbonate≤5ppm, ammonium≤30ppm, water-insoluble
≤ 0.01%, organic matter≤1ppm.
(3) beneficial effect
Compared with prior art, the present invention provides a kind of preparation method of fused salt chlorimation potassium, have following
The utility model has the advantages that
The preparation method of the fused salt chlorimation potassium by potassium chloride dissolving powder, production solution A, refilters to obtain solution B, again
Solution C is made, finally solution C is evaporated under reduced pressure, decrease temperature crystalline obtains wet potassium chloride, then by wet potassium chloride high-temperature calcination
Fused salt chlorimation potassium is purified to obtain, current China's fused salt chlorimation potassium extractive technique is solved and falls behind, the country is used for the chlorination of molten salt system
The problem of potassium relies primarily on import, expensive, and country will spend a large amount of foreign exchanges every year.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution in the embodiment of the present invention is clearly and completely retouched
It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention
In embodiment, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, shall fall within the protection scope of the present invention.
A kind of preparation method of fused salt chlorimation potassium, comprising the following steps:
S1, potassium chloride dissolving powder
1000 milliliters of cold water are taken, 40 DEG C -90 DEG C, then 250-350 grams of potassium chloride powder is heated to, potassium chloride powder is added
Enter and dissolved at 40 DEG C -90 DEG C, produces the Klorvess Liquid that mass concentration is 25%~35%.
Potassium chloride is industry or agricultural potassium chloride in step S1, and when dissolution can be stirred using agitating device, is accelerated
Dissolution, 40 DEG C -90 DEG C of the solution temperature of potassium chloride, further preferably 50 DEG C~60 DEG C, temperature is too low, potassium chloride solubility drop
It is low, increase the steam consumption of subsequent evaporation, increases production cost；Temperature is excessively high, and the organic matter in raw material potassium chloride largely dissolves,
It is unfavorable for post-processing.Klorvess Liquid mass concentration 25%-35%, further preferably 29%~30%, concentration is lower, increases
The steam consumption for adding subsequent evaporation to crystallize increases production cost；Excessive concentration easily leads to line clogging, is unfavorable for the steady of production
It is fixed.
S2, production solution A
It is that excessive barium chloride solution is added in 25%~35% Klorvess Liquid to the resulting concentration of step S1, makes sulfuric acid
Radical ion precipitating, filters to obtain solution A.
Excessive barium chloride solution is added in step S2 into Klorvess Liquid, excessive is 2%-6%, further preferably
3%~5%.
S3, production solution B
Excessive potassium carbonate and potassium hydroxide solution are added into step S2 acquired solution A, makes calcium chloride, magnesium chloride and chlorination
Precipitated barium filters to obtain solution B.
Excessive potassium carbonate and potassium hydroxide solution are added in step S3, is excessively 3%~5%, further preferably carbon
Sour potassium 2%~4%, potassium hydroxide 3%~5%.Additional amount is very few, cannot make the calcium chloride in solution A, and magnesium chloride is sufficiently formed
Precipitating and ammonium chloride decompose；Additional amount is excessive, increases the difficulty of filtering, is unfavorable for subsequent production.
S4, production solution C
Excessive hydrochloric acid is added into step S3 acquired solution B, converts potassium chloride for excessive potassium carbonate, obtains solution C.
It is food grade hydrochloric acid that hydrochloric acid is added in step S4, and salt excessive acid 2%~5% is added；Further preferably 3%-
4%；The very few carbonate that cannot sufficiently remove in solution of additional amount, the excessive PH that cannot be guaranteed product of additional amount.
S5, the wet potassium chloride of production
Acquired solution C in step S4 is evaporated under reduced pressure, decrease temperature crystalline obtains wet potassium chloride.
It is evaporated under reduced pressure in step S5 and refers to that vacuum degree cools down knot in (- 0.080MPa)~(- 0.085MPa), step S5
Crystalline substance, cooling rate be 1-3 DEG C/min, further preferably 1 DEG C -2 DEG C；The too fast products obtained therefrom potassium chloride granularity of cooling rate compared with
Small, cooling rate is unfavorable for the removal of sodium chloride slowly excessively.
S6, purification
Wet potassium chloride high-temperature calcination obtained by step S5 is purified into obtain fused salt chlorimation potassium.
Step S6 high temperature calcining purification temperature is at 300 DEG C~600 DEG C, further preferably 350 DEG C~400 DEG C；Calcining
The burning time is 20~40min, further preferably 30~35min.It further increases calcination temperature and extends calcination time, calcination
Weightlessness does not have significant change, waste of energy.Gained potassium chloride, content >=99.8%, calcination loss≤0.05% in step S6
(500 DEG C, 2hr), calcium≤5ppm, magnesium≤5ppm, sodium≤30ppm, sulfate≤5ppm, carbonate≤5ppm, ammonium≤30ppm,
Water-insoluble≤0.01%, organic matter≤1ppm.
A kind of embodiment one: preparation method of fused salt chlorimation potassium, comprising the following steps:
S1, potassium chloride dissolving powder
1000 milliliters of cold water are taken, 40 DEG C, then 250 grams of potassium chloride powder are heated to, potassium chloride powder is added at 40 DEG C
The Klorvess Liquid that mass concentration is 25% is produced in dissolution；
S2, production solution A
Excessive 2% barium chloride solution is added in gained Klorvess Liquid into step S1, precipitates sulfate ion, mistake
Filter to obtain solution A.
S3, production solution B
Excessive 2% potassium carbonate and excessive 3% potassium hydroxide solution are added into step S2 acquired solution A, makes calcium chloride,
Magnesium chloride and chlorination precipitated barium, filter to obtain solution B.
S4, production solution C
Excessive 2% food grade hydrochloric acid is added into step S3 acquired solution B, removes excessive K2CO3, obtains solution C.
S5, the wet potassium chloride of production
Step S4 acquired solution C is evaporated under reduced pressure at vacuum degree -0.08MPa, with the cooling knot of the cooling rate of 1 DEG C/min
Crystalline substance obtains wet potassium chloride.
S6, purification
Potassium chloride obtained by step S5 is calcined into 40min at 300 DEG C, then through cooling finished product potassium chloride.
A kind of embodiment two: preparation method of fused salt chlorimation potassium, comprising the following steps:
S1, potassium chloride dissolving powder
1000 milliliters of cold water are taken, 50 DEG C, then 290 grams of potassium chloride powder are heated to, potassium chloride powder is added at 50 DEG C
The Klorvess Liquid that mass concentration is 29% is produced in dissolution.
S2, production solution A
Excessive 3% barium chloride solution is added into Klorvess Liquid obtained by step S1, precipitates sulfate ion, filters
Obtain solution A.
S3, production solution B
Excessive 3% potassium carbonate and excessive 4% potassium hydroxide solution are added into step S2 acquired solution A, makes calcium chloride,
Magnesium chloride and chlorination precipitated barium, filter to obtain solution B.
S4, production solution C
Excessive 3% food grade hydrochloric acid is added into step S3 acquired solution B, removes excessive K2CO3, obtains solution C.
S5, the wet potassium chloride of production
Step S4 acquired solution C is passed through at vacuum degree -0.082MPa and is evaporated under reduced pressure, it is cold with the cooling rate of 2 DEG C/min
But it crystallizes, obtains potassium chloride.
S6, purification
Potassium chloride obtained by step S5 is calcined into 30min at 350 DEG C, then through cooling finished product potassium chloride.
A kind of embodiment three: preparation method of fused salt chlorimation potassium, comprising the following steps:
S1, potassium chloride dissolving powder
1000 milliliters of cold water are taken, 60 DEG C, then 300 grams of potassium chloride powder are heated to, potassium chloride powder is added at 60 DEG C
The Klorvess Liquid that mass concentration is 30% is produced in dissolution.
S2, production solution A
Excessive 5% barium chloride solution is added into Klorvess Liquid obtained by step S1, precipitates sulfate ion, filters
Obtain solution A.
S3, production solution B
Excessive 4% potassium carbonate and excessive 5% potassium hydroxide solution are added into step S2 acquired solution A, makes calcium chloride,
Magnesium chloride and chlorination precipitated barium, filter to obtain solution B.
S4, production solution C
Excessive 4% food grade hydrochloric acid is added into step S3 acquired solution B, removes excessive K2CO3, obtains solution C.
S5, the wet potassium chloride of production
Step S4 acquired solution C is passed through and is evaporated under reduced pressure in vacuum degree -0.085MPa, it is cooling with the cooling rate of 3 DEG C/min
Crystallization, obtains potassium chloride.
S6, purification
Potassium chloride obtained by step S5 is calcined into 20min at 400 DEG C, then through cooling finished product potassium chloride.
The beneficial effects of the present invention are: the preparation method of the fused salt chlorimation potassium, passes through potassium chloride dissolving powder, production solution
A, refilter solution B, make solution C again, finally solution C is evaporated under reduced pressure, decrease temperature crystalline obtains wet potassium chloride, then will be wet
Potassium chloride high-temperature calcination purifies to obtain fused salt chlorimation potassium, solves current China's fused salt chlorimation potassium extractive technique and falls behind, domestic
The problem of potassium chloride for molten salt system relies primarily on import, expensive, and country will spend a large amount of foreign exchanges every year.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (8)
1. a kind of preparation method of fused salt chlorimation potassium, which comprises the following steps:
S1, potassium chloride dissolving powder
1000 milliliters of cold water are taken, 40 DEG C -90 DEG C, then 250-350 grams of potassium chloride powder are heated to, potassium chloride powder is added 40
It is dissolved at DEG C -90 DEG C, produces the Klorvess Liquid that mass concentration is 25%~35%；
S2, production solution A
It is that excessive barium chloride solution is added in 25%~35% Klorvess Liquid to the resulting concentration of step S1, makes sulfuric acid
Radical ion precipitating, filters to obtain solution A；
S3, production solution B
Excessive potassium carbonate and potassium hydroxide solution are added into the step S2 acquired solution A, makes calcium chloride, magnesium chloride and chlorination
Precipitated barium filters to obtain solution B；
S4, production solution C
Excessive hydrochloric acid is added into the step S3 acquired solution B, converts potassium chloride for excessive potassium carbonate, obtains solution C；
S5, the wet potassium chloride of production
Acquired solution C in the step S4 is evaporated under reduced pressure, decrease temperature crystalline obtains wet potassium chloride.
S6, purification
Wet potassium chloride high-temperature calcination obtained by the step S5 is purified into obtain fused salt chlorimation potassium.
2. the preparation method of fused salt chlorimation potassium according to claim 1, it is characterised in that: chlorination described in the step S1
Potassium is industry or agricultural potassium chloride, and when dissolution can be stirred using agitating device, accelerates dissolution.
3. the preparation method of fused salt chlorimation potassium according to claim 1, it is characterised in that: be added described in the step S2
Barium chloride be excessively 2%-6%.
4. the preparation method of fused salt chlorimation potassium according to claim 1, it is characterised in that: be added described in the step S3
Potassium carbonate and potassium hydroxide excessive 3%~5%.
5. the preparation method of fused salt chlorimation potassium according to claim 1, it is characterised in that: be added described in the step S4
Hydrochloric acid be excessive 2%~5% food grade hydrochloric acid.
6. the preparation method of fused salt chlorimation potassium according to claim 1, it is characterised in that: be evaporated under reduced pressure in the step S5
Refer to vacuum degree decrease temperature crystalline in (- 0.080MPa)~(- 0.085MPa), step S5,1-3 DEG C of cooling rate/min.
7. the preparation method of fused salt chlorimation potassium according to claim 1, it is characterised in that: the step S6 high temperature calcining
Purification, calcination temperature is at 300-600 DEG C, and calcination time is in 20~40min.
8. the preparation method of fused salt chlorimation potassium according to claim 1, it is characterised in that: gained chlorination in the step S6
Potassium, content >=99.8%, calcination loss≤0.05% (500 DEG C, 2hr), calcium≤5ppm, magnesium≤5ppm, sodium≤30ppm, sulfuric acid
Salt≤5ppm, carbonate≤5ppm, ammonium≤30ppm, water-insoluble≤0.01%, organic matter≤1ppm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111533141A (en) * | 2020-05-20 | 2020-08-14 | 成都华融化工有限公司 | Reagent potassium chloride and preparation method thereof |
| CN114620747A (en) * | 2020-12-10 | 2022-06-14 | 自然资源部天津海水淡化与综合利用研究所 | Method for recycling clodinafop-propargyl byproduct salt |
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| CN102476811A (en) * | 2010-11-24 | 2012-05-30 | 江苏省勤奋药业有限公司 | Production process of large-particle sodium chloride for medicine |
| CN102476812A (en) * | 2010-11-24 | 2012-05-30 | 江苏省勤奋药业有限公司 | Production process of medicinal potassium chloride |
| CN102476813A (en) * | 2010-11-24 | 2012-05-30 | 江苏省勤奋药业有限公司 | Production process of medical large-particle potassium chloride |
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Patent Citations (4)
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|---|---|---|---|---|
| CN1857303A (en) * | 2006-04-04 | 2006-11-08 | 山东肥城精制盐厂 | Preparing method of sodium chloride for sheet injection |
| CN102476811A (en) * | 2010-11-24 | 2012-05-30 | 江苏省勤奋药业有限公司 | Production process of large-particle sodium chloride for medicine |
| CN102476812A (en) * | 2010-11-24 | 2012-05-30 | 江苏省勤奋药业有限公司 | Production process of medicinal potassium chloride |
| CN102476813A (en) * | 2010-11-24 | 2012-05-30 | 江苏省勤奋药业有限公司 | Production process of medical large-particle potassium chloride |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111533141A (en) * | 2020-05-20 | 2020-08-14 | 成都华融化工有限公司 | Reagent potassium chloride and preparation method thereof |
| CN114620747A (en) * | 2020-12-10 | 2022-06-14 | 自然资源部天津海水淡化与综合利用研究所 | Method for recycling clodinafop-propargyl byproduct salt |
| CN114620747B (en) * | 2020-12-10 | 2023-09-19 | 自然资源部天津海水淡化与综合利用研究所 | Method for recycling clodinafop-propargyl byproduct salt |
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