CN106586990A - Method of using phosphoric acid by wet process to produce monopotassium phosphate - Google Patents
Method of using phosphoric acid by wet process to produce monopotassium phosphate Download PDFInfo
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- CN106586990A CN106586990A CN201610988560.1A CN201610988560A CN106586990A CN 106586990 A CN106586990 A CN 106586990A CN 201610988560 A CN201610988560 A CN 201610988560A CN 106586990 A CN106586990 A CN 106586990A
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- phosphoric acid
- dihydrogen phosphate
- potassium dihydrogen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
- C01B25/301—Preparation from liquid orthophosphoric acid or from an acid solution or suspension of orthophosphates
- C01B25/303—Preparation from liquid orthophosphoric acid or from an acid solution or suspension of orthophosphates with elimination of impurities
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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
Abstract
The invention discloses a method of using phosphoric acid by a wet process to produce monopotassium phosphate. The method comprises the steps of adding phosphoric ore pulp and barium carbonate into phosphoric acid by the wet process sequentially so as to reduce the concentration of sulfate ion in phosphoric acid to 0.5g/L, conducting still standing and sedimentation and then taking supernatant liquid as fine desulfurization dilute phosphoric acid, using a compound extraction agent obtained by mixing octylame and octanol according to a random ratio to extract the fine desulfurization dilute phosphoric acid, and conducting still standing and phase splitting, wherein an organic phase of the coupling phosphoric acid is extract liquor and the residual phosphoric acid is raffinate; adding potassium chloride into the extract liquor to be subjected to reaction, and conducting still standing and phase splitting, wherein the lower layer is a monopotassium phosphate thick solution and the upper layer is the organic phase which is rich in hydrochloric acid and a small amount of phosphoric acid and potassium chloride; filtrating the monopotassium phosphate thick solution, afterwards, adding potassium hydroxide into filter liquor to adjust pH of the solution to be about 6, conducting still standing and sedimentation, and afterwards, removing impurities to obtain a monopotassium phosphate refined solution; adding purified phosphoric acid into the monopotassium phosphate refined solution to adjust the pH to be 4-5, and conducting concentration, crystallization, filtration and drying on the monopotassium phosphate refined solution to obtain a monopotassium phosphate product. The technological process is simple and the cost is low.
Description
Technical field
The present invention relates to a kind of method of use Wet-process Phosphoric Acid Production potassium dihydrogen phosphate, belongs to solvent extraction production di(2-ethylhexyl)phosphate
Hydrogen potassium technique.
Background technology
Potassium dihydrogen phosphate has extensive purposes in industrial and agricultural production.Industrially it is used as buffer, hardening agent, flavor enhancement
Deng.Agriculturally potassium dihydrogen phosphate is high concentration phosphorus potash fertilizer, obvious to increasing crop yield the effect of increasing income.Potassium dihydrogen phosphate or full water
Dissolubility efficiently sprays fertilizer, be widely used in spray, dropper system.
At present, the production method of potassium dihydrogen phosphate mainly has neutralisation, double decomposition, solvent extraction etc..The country adopts
Solvent extraction produces the technological process of potassium dihydrogen phosphate：Phosphoric acid by wet process desulfurization, defluorinate, then organic solvent extracting and purifying is used,
The extraction acid sludge that purification process is produced is used for producing fertilizer；Phosphoric acid after purification adds potassium chloride solution and organic solvent to carry out
Extract and separate, the aqueous solution for potassium dihydrogen phosphate solution, concentrate drying after potassium dihydrogen phosphate product, rich in the organic of chlorion
Communicating organic phase after ammonia back extraction can obtain N P and K NPK as extractant recycling, aqueous solution concentrate drying.Should
Method is needed using two kinds of organic solvents, there is the extraction process in two stages, and operation cost is high.
Have in addition and be purified after acid using phosphoric acid by wet process solvent extraction, with ammonia and to obtain ammonium dihydrogen phosphate molten
Liquid, potassium chloride is added afterwards carries out metathesis reaction.The potassium dihydrogen phosphate product purity that the method is obtained is not fine, needs two
Secondary crystallization.
As can be seen here, prior art all exist removal of impurities not thoroughly, mother liquor can not be utilized rationally, extractant consumes many,
So that phosphrus reagent is low, production cost increases, these are all this area problem demanding prompt solutions.
The content of the invention
For existing problem, it is an object of the invention to provide a kind of side of use Wet-process Phosphoric Acid Production potassium dihydrogen phosphate
Method, low production cost, process is simple, Impurity removal are thorough.
To achieve these goals, the technical scheme is that such：One kind uses Wet-process Phosphoric Acid Production biphosphate
The method of potassium, comprises the steps：
A, the addition phosphate ore pulp reaction in phosphoric acid by wet process, the concentration for making sulfate ion in phosphoric acid is down to below 8g/L, quiet
Put and take after sedimentation supernatant liquor acid；
B, in supernatant liquor acid brium carbonate is added to continue to react, the concentration for making sulfate ion in phosphoric acid is down to 0.5g/
L, it is fine de-sulfur phosphoric acid,diluted that supernatant liquor acid is taken after standing sedimentation；
C, the above-mentioned fine de-sulfur phosphoric acid,diluted of composite extractant extraction mixed according to arbitrary proportion with octylame and octanol, it is quiet
Split-phase is put, the organic phase for coupling phosphoric acid is extract, remaining phosphoric acid is raffinate；
D, in above-mentioned extract add potassium chloride reacted, stand split-phase, lower floor be the thick solution of potassium dihydrogen phosphate, on
Layer is the organic phase rich in hydrochloric acid and a small amount of phosphoric acid and potassium chloride；
After the thick solution of potassium dihydrogen phosphate is filtered in e, step d, add potassium hydroxide to adjust pH value of solution in filtrate and be about 6,
Impurity is filtered off after standing sedimentation and obtains potassium dihydrogen phosphate essence solution；
f：Purifying phosphoric acid is added to adjust pH for 4-5 in above-mentioned potassium dihydrogen phosphate essence solution, resulting solution condensing crystallizing, mistake
Filter, be dried to obtain potassium dihydrogen phosphate product, filtrate is potassium dihydrogen phosphate mother liquor.
Using such scheme, increasing step a and b can play a part of sulfate radical, and sulfate radical foreign matter is removed more
Thoroughly, using octylame and octanol double solvents as extractant, octylame is alkalescence to step c, and (fluorine is in alkali to play fluorine removal and chlorine
Property under the conditions of can and cation complex, generate the precipitation such as fluosilicic acid iron aluminium), reduce defluorinate operation, reduces cost.Using compound
Extractant elder generation enrichment acid, removes again hydrochloric acid after mixing with potassium chloride afterwards, only extraction once, reduces production cost, secondly,
The quality of raffinate is little compared with ortho acid change, alleviates follow-up ammonium phosphate production system load.
In such scheme：Composite extractant and fine de-sulfur phosphoric acid,diluted is in a ratio of 1 in step c:2—1；Between 4, reaction temperature
Spend for 50-70 DEG C, the reaction time is 30-40min.
In such scheme, in the composite extractant, the volume ratio of octylame and octanol is 6:4-8:1.Can meet enough
Octylame participates in reaction.
In such scheme, potassium chloride and P in extract in step d2O5Mol ratio between 1.03-1.05, reaction temperature
Spend for 50-70 DEG C, the reaction time is 20-40min.
In such scheme, P in the raffinate in step c2O5Content is about 18-20%, is subsequently used for phosphorus ammonium or slurry-spraying pelletizing
The production of composite fertilizer.The quality of raffinate is little compared with ortho acid change, alleviates follow-up ammonium phosphate production system load.
In such scheme, ammoniacal liquor is added to adjust in the organic phase in step d rich in hydrochloric acid and a small amount of phosphoric acid and potassium chloride
PH is 7-8, and reaction temperature is 50-70 DEG C, and the reaction time is 20-40min, stands split-phase, and lower floor's liquid is concentrated to give N P and K three
Component composite fertilizer byproduct；Upper strata is extractant phase, is recycled as the extractant in step c.
In such scheme：Carry out extracting the reaction of split-phase in potassium dihydrogen phosphate mother liquor return to step d in step f.
The invention has the beneficial effects as follows：Compared with prior art, invention increases the desulfurization process of step a and b so that
The removing of sulfate radical foreign matter is more thorough in products obtained therefrom of the present invention；Composite extractant of the present invention comes first enrichment acid, Zhi Houyu
Remove hydrochloric acid again after potassium chloride mixing, only need to extract once, reduce the use of phosphoric acid purification extractant, reduce and produce into
This；And raffinate quality is little compared with ortho acid change, alleviates the load of follow-up ammonium phosphate production system；Again, using compound extraction
When taking agent extraction, fluorine ion is also separated with precipitation form from the solution of potassium dihydrogen phosphate, reduces defluorinate operation, further
Reduce into product cost.The good product quality for obtaining.
Specific embodiment
With reference to specific embodiment, the present invention will be further described：
Embodiment 1
A kind of method of use Wet-process Phosphoric Acid Production potassium dihydrogen phosphate, completes in accordance with the following steps：
A, in 1000kg phosphoric acid by wet processes add 50kg moistures be 35% phosphate ore pulp, the stirring reaction at 80 DEG C
2h, the concentration for making sulfate ion in phosphoric acid is down to below 8g/L, and supernatant liquor acid is taken after standing sedimentation.
B, in the acid of 800kg supernatant liquors 13.8kg brium carbonates are added, the concentration for making sulfate ion in phosphoric acid is down to
0.5g/L, it is fine de-sulfur phosphoric acid,diluted that supernatant liquor acid is taken after standing sedimentation.
C, with octylame and octanol according to volume ratio 4:It is dilute that the composite extractant that 1 ratio is mixed extracts above-mentioned fine de-sulfur
Phosphoric acid, composite extractant is 1 with the volume ratio of fine de-sulfur phosphoric acid,diluted:2, reaction temperature is 50 DEG C, and the reaction time is 30min, quiet
The split-phase time is put for 20-30min.The organic phase of coupling phosphoric acid is extract, and remaining phosphoric acid is raffinate.P in raffinate2O5Contain
Amount is about 18-20%, is subsequently used for the production of phosphorus ammonium or slurry-spraying pelletizing composite fertilizer.
D, in above-mentioned extract Klorvess Liquid is added to be reacted, the volume ratio of extract and Klorvess Liquid is 2:
1, P in potassium chloride and extract2O5Mol ratio be 1.03, reaction temperature be 50 DEG C, the reaction time is 40min, stand split-phase when
Between for 20-30min lower floors be the thick solution of potassium dihydrogen phosphate, upper strata be the organic phase rich in hydrochloric acid and a small amount of phosphoric acid and potassium chloride.
It is 7-8 to add ammoniacal liquor to adjust pH in organic phase rich in hydrochloric acid and a small amount of phosphoric acid and potassium chloride, and reaction temperature is 50-70 DEG C, instead
It is 20-40min between seasonable, stands split-phase, lower floor's liquid is concentrated to give N P and K NPK byproduct；Upper strata is extractant
Phase, recycles as the extractant in step c.
After the thick solution of potassium dihydrogen phosphate is filtered in e, step d, add potassium hydroxide to adjust pH value of solution in filtrate and be about 6,
Impurity is filtered off after standing sedimentation and obtains potassium dihydrogen phosphate essence solution.
f：It is 4 to add purifying phosphoric acid to adjust pH in above-mentioned potassium dihydrogen phosphate essence solution, and resulting solution condensing crystallizing is crossed and is filtered dry
Dry to obtain potassium dihydrogen phosphate product, filtrate is potassium dihydrogen phosphate mother liquor.Extraction point is carried out in potassium dihydrogen phosphate mother liquor return to step d
The reaction of phase.
Survey P in gained potassium dihydrogen phosphate product2O5Content is 51.06%, K2O content is 33.9%.
Embodiment 2
A kind of method of use Wet-process Phosphoric Acid Production potassium dihydrogen phosphate, completes in accordance with the following steps：
A, in 1000kg phosphoric acid by wet processes add 50kg moistures be 35% phosphate ore pulp, the stirring reaction at 80 DEG C
2h, the concentration for making sulfate ion in phosphoric acid is down to below 8g/L, and supernatant liquor acid is taken after standing sedimentation.
B, in the acid of 800kg supernatant liquors 13.8kg brium carbonates are added, the concentration for making sulfate ion in phosphoric acid is down to
0.5g/L, it is fine de-sulfur phosphoric acid,diluted that supernatant liquor acid is taken after standing sedimentation.
C, with octylame and octanol according to volume ratio 8:It is dilute that the composite extractant that 1 ratio is mixed extracts above-mentioned fine de-sulfur
Phosphoric acid, composite extractant is 1 with the volume ratio of fine de-sulfur phosphoric acid,diluted:4, reaction temperature is 70 DEG C, and the reaction time is 40min, quiet
The split-phase time is put for 20-30min.The organic phase of coupling phosphoric acid is extract, and remaining phosphoric acid is raffinate.P in raffinate2O5Contain
Amount is about 18-20%, is subsequently used for the production of phosphorus ammonium or slurry-spraying pelletizing composite fertilizer.
D, in above-mentioned extract Klorvess Liquid is added to be reacted, the volume ratio of extract and Klorvess Liquid is 2:
1, P in potassium chloride and extract2O5Mol ratio be 1.05, reaction temperature be 70 DEG C, the reaction time is 20min, stand split-phase when
Between for 20-30min lower floors be the thick solution of potassium dihydrogen phosphate, upper strata be the organic phase rich in hydrochloric acid and a small amount of phosphoric acid and potassium chloride.
It is 7-8 to add ammoniacal liquor to adjust pH in organic phase rich in hydrochloric acid and a small amount of phosphoric acid and potassium chloride, and reaction temperature is 50-70 DEG C, instead
It is 20-40min between seasonable, stands split-phase, lower floor's liquid is concentrated to give N P and K NPK byproduct；Upper strata is extractant
Phase, recycles as the extractant in step c.
After the thick solution of potassium dihydrogen phosphate is filtered in e, step d, add potassium hydroxide to adjust pH value of solution in filtrate and be about 6,
Impurity is filtered off after standing sedimentation and obtains potassium dihydrogen phosphate essence solution.
f：It is 5 to add purifying phosphoric acid to adjust pH in above-mentioned potassium dihydrogen phosphate essence solution, and resulting solution condensing crystallizing is crossed and is filtered dry
Dry to obtain potassium dihydrogen phosphate product, filtrate is potassium dihydrogen phosphate mother liquor.Extraction point is carried out in potassium dihydrogen phosphate mother liquor return to step d
The reaction of phase.
Survey P in gained potassium dihydrogen phosphate product2O5Content is 50.28%, K2O content is 32.89%.
Embodiment 3
A kind of method of use Wet-process Phosphoric Acid Production potassium dihydrogen phosphate, completes in accordance with the following steps：
A, in 1000kg phosphoric acid by wet processes add 50kg moistures be 35% phosphate ore pulp, the stirring reaction at 80 DEG C
2h, the concentration for making sulfate ion in phosphoric acid is down to below 8g/L, and supernatant liquor acid is taken after standing sedimentation.
B, in the acid of 800kg supernatant liquors 13.8kg brium carbonates are added, the concentration for making sulfate ion in phosphoric acid is down to
0.5g/L, it is fine de-sulfur phosphoric acid,diluted that supernatant liquor acid is taken after standing sedimentation.
C, with octylame and octanol according to volume ratio 6：It is dilute that the composite extractant that 4 ratio is mixed extracts above-mentioned fine de-sulfur
Phosphoric acid, composite extractant is 1 with the volume ratio of fine de-sulfur phosphoric acid,diluted:3, reaction temperature is 60 DEG C, and the reaction time is 30min, quiet
The split-phase time is put for 20-30min.The organic phase of coupling phosphoric acid is extract, and remaining phosphoric acid is raffinate.P in raffinate2O5Contain
Amount is about 18-20%, is subsequently used for the production of phosphorus ammonium or slurry-spraying pelletizing composite fertilizer.
D, in above-mentioned extract Klorvess Liquid is added to be reacted, the volume ratio of extract and Klorvess Liquid is 2:
1, P in potassium chloride and extract2O5Mol ratio be 1.04, reaction temperature be 60 DEG C, the reaction time is 30min, stand split-phase when
Between for 20-30min lower floors be the thick solution of potassium dihydrogen phosphate, upper strata be the organic phase rich in hydrochloric acid and a small amount of phosphoric acid and potassium chloride.
It is 7-8 to add ammoniacal liquor to adjust pH in organic phase rich in hydrochloric acid and a small amount of phosphoric acid and potassium chloride, and reaction temperature is 50-70 DEG C, instead
It is 20-40min between seasonable, stands split-phase, lower floor's liquid is concentrated to give N P and K NPK byproduct；Upper strata is extractant
Phase, recycles as the extractant in step c.
After the thick solution of potassium dihydrogen phosphate is filtered in e, step d, add potassium hydroxide to adjust pH value of solution in filtrate and be about 6,
Impurity is filtered off after standing sedimentation and obtains potassium dihydrogen phosphate essence solution.
f：It is 4.5 to add purifying phosphoric acid to adjust pH in above-mentioned potassium dihydrogen phosphate essence solution, and resulting solution condensing crystallizing is filtered
Potassium dihydrogen phosphate product is dried to obtain, filtrate is potassium dihydrogen phosphate mother liquor.Extracted in potassium dihydrogen phosphate mother liquor return to step d
The reaction of split-phase.
Survey P in gained potassium dihydrogen phosphate product2O5Content is 51.32%, K2O content is 33.29%.
The present invention is not limited to above-mentioned specific embodiment, it will be appreciated that one of ordinary skill in the art is without the need for creative
Work just can make many modifications and variations with design of the invention.In a word, all technical staff in the art are according to this
The design of invention passes through on the basis of existing technology the available technical side of logical analysis, reasoning, or a limited experiment
Case, all should be in the protection domain being defined in the patent claims.
Claims (7)
1. a kind of method of use Wet-process Phosphoric Acid Production potassium dihydrogen phosphate, comprises the steps：
A, the addition phosphate ore pulp reaction in phosphoric acid by wet process, the concentration for making sulfate ion in phosphoric acid is down to below 8g/L, and it is heavy to stand
Supernatant liquor acid is taken after drop；
B, to supernatant liquor acid in add brium carbonate continue react, the concentration for making sulfate ion in phosphoric acid is down to 0.5g/L, quiet
It is fine de-sulfur phosphoric acid,diluted to put and take after sedimentation supernatant liquor acid；
C, the above-mentioned fine de-sulfur phosphoric acid,diluted of composite extractant extraction mixed according to arbitrary proportion with octylame and octanol, stand and divide
Phase, the organic phase for coupling phosphoric acid is extract, and remaining phosphoric acid is raffinate；
D, in above-mentioned extract add potassium chloride to be reacted, stand split-phase, lower floor is that the thick solution of potassium dihydrogen phosphate, upper strata are
Organic phase rich in hydrochloric acid and a small amount of phosphoric acid and potassium chloride；
After the thick solution of potassium dihydrogen phosphate is filtered in e, step d, add potassium hydroxide to adjust pH value of solution in filtrate and be about 6, stand
Impurity is filtered off after sedimentation and obtains potassium dihydrogen phosphate essence solution；
f：To above-mentioned potassium dihydrogen phosphate essence solution in plus purifying phosphoric acid adjust pH be 4-5, resulting solution condensing crystallizing, filtrations, do
Dry to obtain potassium dihydrogen phosphate product, filtrate is potassium dihydrogen phosphate mother liquor.
2. according to claim 1 with the method for Wet-process Phosphoric Acid Production potassium dihydrogen phosphate, it is characterised in that：It is combined in step c
Extractant is in a ratio of 1 with fine de-sulfur phosphoric acid,diluted:2—1：Between 4, reaction temperature is 50-70 DEG C, and the reaction time is 30-
40min。
3. the method for use Wet-process Phosphoric Acid Production potassium dihydrogen phosphate according to claim 1 or claim 2, it is characterised in that：It is described compound
In extractant, the volume ratio of octylame and octanol is 6:4-8:1.
4. the method for use Wet-process Phosphoric Acid Production potassium dihydrogen phosphate according to claim 1 or claim 2, it is characterised in that：
Potassium chloride and P in extract in step d2O5Mol ratio between 1.03-1.05, reaction temperature be 50-70 DEG C, reaction
Time is 20-40min.
5. the method for use Wet-process Phosphoric Acid Production potassium dihydrogen phosphate according to claim 1 or claim 2, it is characterised in that：In step c
P in raffinate2O5Content is about 18-20%, is subsequently used for the production of phosphorus ammonium or slurry-spraying pelletizing composite fertilizer.
6. according to claim 5 with the method for Wet-process Phosphoric Acid Production potassium dihydrogen phosphate, it is characterised in that：It is rich in step d
It is 7-8 to add ammoniacal liquor to adjust pH in the organic phase of hydrochloric and a small amount of phosphoric acid and potassium chloride, and reaction temperature is 50-70 DEG C, reaction
Time is 20-40min, stands split-phase, and lower floor's liquid is concentrated to give N P and K NPK byproduct；Upper strata is extractant phase,
Recycle as the extractant in step c.
7. according to claim 6 with the method for Wet-process Phosphoric Acid Production potassium dihydrogen phosphate, it is characterised in that：Phosphorus in step f
Carry out extracting the reaction of split-phase in acid dihydride potassium mother liquor return to step d.
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| CN107758637A (en) * | 2017-11-13 | 2018-03-06 | 贵阳开磷化肥有限公司 | A kind of method of the micro- reaction production PHOSPHORIC ACID TECH.GRADE potassium dihydrogen of phosphoric acid by wet process |
| CN113415791A (en) * | 2021-06-25 | 2021-09-21 | 云南云天化红磷化工有限公司 | Device and method for recovering extractant in production of monopotassium phosphate by wet-process phosphoric acid extraction |
| CN114191847A (en) * | 2021-12-12 | 2022-03-18 | 四川鑫瑞源科技发展有限公司 | Extracting agent for producing potassium dihydrogen phosphate by solvent extraction method and preparation method and application thereof |
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| CN105000539A (en) * | 2015-08-17 | 2015-10-28 | 四川大学 | Method for producing potassium dihydrogen phosphate and potassium-ammonium dihydrogen phosphate through wet process phosphoric acid |
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| CN107758637A (en) * | 2017-11-13 | 2018-03-06 | 贵阳开磷化肥有限公司 | A kind of method of the micro- reaction production PHOSPHORIC ACID TECH.GRADE potassium dihydrogen of phosphoric acid by wet process |
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| CN113415791A (en) * | 2021-06-25 | 2021-09-21 | 云南云天化红磷化工有限公司 | Device and method for recovering extractant in production of monopotassium phosphate by wet-process phosphoric acid extraction |
| CN113415791B (en) * | 2021-06-25 | 2022-11-29 | 云南云天化红磷化工有限公司 | Device and method for recovering extractant in production of monopotassium phosphate by wet-process phosphoric acid extraction |
| CN114191847A (en) * | 2021-12-12 | 2022-03-18 | 四川鑫瑞源科技发展有限公司 | Extracting agent for producing potassium dihydrogen phosphate by solvent extraction method and preparation method and application thereof |
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| CN106586990B (en) | 2019-03-19 |
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