CN108609592A - The method of Purification of Wet process Phosphoric Acid by Solvent Extraction coproduction potassium dihydrogen phosphate - Google Patents
The method of Purification of Wet process Phosphoric Acid by Solvent Extraction coproduction potassium dihydrogen phosphate Download PDFInfo
- Publication number
- CN108609592A CN108609592A CN201810725232.1A CN201810725232A CN108609592A CN 108609592 A CN108609592 A CN 108609592A CN 201810725232 A CN201810725232 A CN 201810725232A CN 108609592 A CN108609592 A CN 108609592A
- Authority
- CN
- China
- Prior art keywords
- phosphoric acid
- washing
- wet process
- organic
- dihydrogen phosphate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
- C01B25/46—Preparation involving solvent-solvent extraction
- C01B25/461—Preparation involving solvent-solvent extraction the phosphoric acid present in the medium obtained after reaction being first extracted from the liquid phase formed or separated then re-extracted as free acid by using water or as a phosphate by using a basic compound
- C01B25/465—Preparation involving solvent-solvent extraction the phosphoric acid present in the medium obtained after reaction being first extracted from the liquid phase formed or separated then re-extracted as free acid by using water or as a phosphate by using a basic compound the extracting agent being an ester or a mixture of esters
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present invention provides a kind of methods of Purification of Wet process Phosphoric Acid by Solvent Extraction coproduction potassium dihydrogen phosphate, include the following steps：(1), the technique that load organic phases are obtained by extraction with compounded organic solvent again after desulfurization defluorinate sedimentation filtration in phosphoric acid by wet process；Or after phosphoric acid by wet process is directly over sedimentation, extracted using compounded organic solvent, then loads addition desulfurization defluorinating agent progress desulfurization defluorinate in the organic phase of phosphoric acid and obtain load organic phases；(2), load organic phases are washed with wet cleaning phosphoric acid,diluted；(3), the load organic phases after washing are washed using the organic phase after deionized water back extraction (4), back extraction using potassium hydroxide solution, and the organic phase after washing, which returns, is used as extractant；(5), purification phosphoric acid,diluted is added in cleaning solution, is filtered after mixing, removes solid organic impurities, adds potassium hydroxide and adjusts pH, concentrate, crystallize, be dried to obtain potassium dihydrogen phosphate.Phenomena such as eliminating index deterioration, the emulsification entrainment that the long-term operation of extractant is brought.
Description
Technical field
The present invention relates to a kind of methods of Purification of Wet process Phosphoric Acid by Solvent Extraction coproduction potassium dihydrogen phosphate, belong to wet method phosphorus
Sour field.
Background technology
Phosphoric acid is one of large chemical products, and commercial run has two kinds of Re Fa and wet method.Thermal phosphoric acid purity is high, main
It is used for chemical industry and food medicine aspect.Phosphoric acid by wet process impurity is more, multi-purpose to make chemical fertilizer aspect.Phosphoric acid by wet process cost specific heat
Method about low 25% or so, the standard for making it to reach technical grade to the exploitation of wet phosphoric acid purifying technology is with very great
Meaning.
Currently, purification of wet process phosphoric acid realizes industrialized only solvent extraction.When using solvent extraction, compound extracting
Solvent (mixture of tributyl phosphate and kerosene) continues to return to extraction stages phosphoric acid extraction after back extraction.With the fortune of device
Row, after reusing several times, composite extractant aging is serious, and emulsification entrainment phenomenon is serious, and extracting power is lower, wet cleaning
Phosphoric acid,diluted index is deteriorated (amount of iron ion can reach 100-200mg/kg, and the amount of sulfate radical is more than 200mg/kg) so that wet method
The standard of industrial phosphoric acid is not achieved in purification phosphoric acid,diluted subsequent processing.Therefore it just needs in use for some time these are compound
Organic extractant is changed, and causes economic loss, and increase the processing cost of Discarded organic solvent.
Invention content
Present invention seek to address that the technical problems existing in the prior art, especially innovatively propose a kind of solvent extraction
The method of method purification of wet process phosphoric acid coproduction potassium dihydrogen phosphate carries out letter before composite extractant returns to extraction to composite extractant
Single washing, so that composite extractant can be reused always, and does not influence the quality of phosphoric acid.
In order to realize the above-mentioned purpose of the present invention, the present invention provides a kind of Purification of Wet process Phosphoric Acid by Solvent Extraction coproduction
The method of potassium dihydrogen phosphate, which is characterized in that including with following processing step：
(1), phosphoric acid by wet process obtains desulfurization defluorinate phosphoric acid by wet process after desulfurization defluorination process sedimentation filtration, then with compound
The process that load organic phases are obtained by extraction in organic solvent；
Or after phosphoric acid by wet process is directly over sedimentation, extracted using compounded organic solvent, then loads the organic of phosphoric acid
Desulfurization defluorinating agent is added in phase and carries out desulfurization defluorinate, then sedimentation, split-phase obtain load organic phases；
The compounded organic solvent is the mixture of tributyl phosphate and kerosene；
(2), the process that load organic phases are washed with wet cleaning phosphoric acid,diluted, the acid after washing are collected spare；
(3), the load organic phases after washing are stripped the process for obtaining wet cleaning phosphoric acid,diluted using deionized water；
(4), the organic phase after being stripped is washed using potassium hydroxide solution, the organic phase after being washed and cleaning solution,
Extractant is used as in organic phase return to step (1) after middle washing；
(5), wet cleaning phosphoric acid,diluted is added in the cleaning solution in step (4), is filtered after mixing, it is organic miscellaneous to remove solid
Matter, then potassium hydroxide is added in filtrate and adjusts pH4-4.5, it concentrates, crystallize, be dried to obtain potassium dihydrogen phosphate product.
Using the above scheme, after load organic oppositing back-extraction takes, organic phase is washed using potassium hydroxide solution,
Organic phase after washing is returned again to as extractant, and compounded organic solvent can be used for a long time, not aging.Wet cleaning phosphoric acid,diluted
With the long-term operation of extractant, index will not deteriorate, and Fe contents can be down to 4-10mg/L, SO4 2-Content can be down to 20-
100mg/L can reach the product index of PHOSPHORIC ACID TECH.GRADE after the simple process such as concentrated.
In said program, in step (1), the technique of desulfurization defluorinate is before extracting：According to parts by weight, in a wet method
0.02-0.03 parts of the thick desulfurization of calcium oxide is added in phosphoric acid, is separated by solid-liquid separation after sedimentation, add in the liquid phase 0.005 part-
0.01 part of barium carbonate and 0.002 part -1 part of sodium hydroxide fine de-sulfur fluorine obtain the dense phosphorus of desulfurization defluorinate wet method by press filtration.
In said program, in step (1), the technique of desulfurization defluorinate is after extraction：After washing in a step (2)
Acid in 0.01-0.02 part of calcium oxide and 0.004-0.008 part of sodium hydroxide is added, fully dissolve after reacting, with 0.2-
The organic phase of 0.4 part of load phosphoric acid, which is stirred, carries out desulfurization defluorination reaction, then settles split-phase, and the acid after split-phase is mutually pressed
It is returned after filter and continues to dissolve calcium oxide and sodium hydroxide, the organic phase after split-phase enters step (2) washing procedure.Using first extracting
It takes, the technique of rear desulfurization defluorinate, the desulfurization defluorinating agent requirement on the one hand used is relatively low, and calcium oxide inexpensively may be used
It is at low cost and de- with sodium hydroxide (first desulfurization defluorinate extracts again to be needed to use barium carbonate, barium carbonate price expensive compared with calcium oxide)
The effect of sulphur defluorinate is with using the effect of barium carbonate in first desulfurization defluorination process, saving great amount of cost.Desulfurization defluorinate is anti-
The condition answered is to react 2-3h at 60-70 DEG C.
In said program, the technique of extraction is：Wet method in every part of desulfurization defluorinate phosphoric acid by wet process or after being directly over sedimentation
2-5 parts of compounded organic solvents are added in phosphoric acid to be extracted.
In said program：Per 10-100 parts of load organic phases with the 1 part of washing of wet cleaning phosphoric acid,diluted in step (2).
In said program：Load organic phases per 8-12 parts after washing are stripped using 1 part of deionized water.
In said program：In step (4), the organic phase per 3-5 parts after back extraction is washed using 1 part of potassium hydroxide solution
It washs.
In said program：The mass concentration of potassium hydroxide solution is 5%-15%.
In said program：In step (5), 1 part of purification phosphoric acid,diluted is added in every 4-6 parts of cleaning solution, is filtered after mixing,
Remove solid organic impurities.
Advantageous effect：A kind of solvent extraction using the present invention produces wet cleaning phosphoric acid,diluted coproduction potassium dihydrogen phosphate
Method, eliminate the index that the long-term operation of extractant is brought deteriorate, serious emulsification entrainment phenomena such as, just by this method
Wet cleaning phosphoric acid,diluted index can be made to stablize, wet cleaning phosphoric acid,diluted can reach the index of industrial phosphoric acid after simple process
It is required that reducing production cost, the amount of organic waste is reduced, the processing cost of organic waste is reduced.And the attached production of the present invention
The potassium dihydrogen phosphate product of high-purity (90-98%), obtains the interests of bigger.
Specific implementation mode
The present invention is described further with reference to embodiment.
Embodiment 1
(1) according to weight, 1 part of P2O5Content is that 0.02 part of calcium oxide is added in the wet method concentrated phosphoric acid of 40% (mass concentration)
Be stirred to react 3h at 60 DEG C and carry out thick desulfurization, after then settling press filtration, added in filtrate 0.005 part barium carbonate and
0.002 part of sodium hydroxide is stirred to react 3h at 60 DEG C and carries out fine de-sulfur defluorinate, and it is dense to obtain desulfurization defluorinate wet method by press filtration
Phosphorus.
By obtained desulfurization defluorinate phosphoric acid by wet process and 2 parts of compounded organic solvents, (tributyl phosphate and kerosene are according to volume ratio
4:1 ratio mixing) hybrid extraction, raffinate after extraction enters other production processes.
(2) 10 parts of the organic phase of extraction back loading phosphoric acid carries out once washing for 1 part with wet cleaning phosphoric acid,diluted, after washing
Acid collect it is spare.
(3) 8 parts of load organic phases after washing, are stripped for 1 part with deionized water, obtain wet cleaning phosphoric acid,diluted, institute
It is 3mg/kg, SO to obtain wet cleaning phosphoric acid,diluted Fe contents4 2-Content is 85mg/kg.
(4) 5 parts of organic phase after being stripped, 1 part of potassium hydroxide solution for being 10% with mass concentration are washed, are obtained
The organic phase after potassium dihydrogen phosphate containing organic impurities and washing after washing, the organic phase after washing enter step (1)
As compound extracting solvent.It reuses always, the index of gained wet cleaning phosphoric acid,diluted is constant.
(5) 1 part of wet cleaning phosphoric acid,diluted, mixing is added in 6 parts of the potassium dihydrogen phosphate containing organic impurities after washing
It is separated by solid-liquid separation afterwards and removes a large amount of solid organic impurities, it is 4-4.5, concentration, knot that potassium hydroxide is added in the liquid phase and adjusts pH
Crystalline substance is dried to obtain potassium dihydrogen phosphate product, product purity 96%.
Embodiment 2
(1) according to weight, 1 part of P2O5Content is that 0.03 part of calcium oxide is added in the wet method concentrated phosphoric acid of 40% (mass concentration)
It is stirred to react 2h at 70 DEG C and carries out thick desulfurization, after then settling press filtration, 0.01 part of barium carbonate and 1 is added in filtrate
The sodium hydroxide of part is stirred to react 3h at 60 DEG C and carries out fine de-sulfur defluorinate, and the dense phosphorus of desulfurization defluorinate wet method is obtained by press filtration.
By obtained desulfurization defluorinate phosphoric acid by wet process and 5 parts of compounded organic solvents, (tributyl phosphate and kerosene are according to volume ratio
4:1 ratio mixing) hybrid extraction, raffinate after extraction enters other production processes.
(2) 50 parts of the organic phase of extraction back loading phosphoric acid is washed for 1 part with wet cleaning phosphoric acid,diluted, the acid after washing
It collects spare.
(3) 10 parts of organic phase after washing, is stripped for 1 part with deionized water, obtains wet cleaning phosphoric acid,diluted, gained
Wet cleaning phosphoric acid,diluted Fe contents are 8mg/kg, SO4 2-Content is 40mg/kg.
(4) 4 parts of organic phase after being stripped is that 1 part of 10% potassium hydroxide solution is washed with mass concentration, is washed
The organic phase after potassium dihydrogen phosphate containing organic impurities and washing after washing, the organic phase after washing enter (1) step into
Row hybrid extraction process.
(5) 1 part of wet cleaning phosphoric acid,diluted, mixing is added in 5 parts of the potassium dihydrogen phosphate containing organic impurities after washing
After be filtered to remove a large amount of solid organic impurities, it is 4-4.5 that filtrate, which adds potassium hydroxide and adjusts pH, concentration, crystallization, dry
Obtain potassium dihydrogen phosphate product, product purity 92%.
Embodiment 3
(1) according to weight, 1 part of P2O5Content is that 0.02 part of calcium oxide is added in the wet method concentrated phosphoric acid of 42% (mass concentration)
Be stirred to react 3h at 60 DEG C and carry out thick desulfurization, after then settling press filtration, added in filtrate 0.008 part barium carbonate and
0.01 part of sodium hydroxide is stirred to react 2h at 70 DEG C and carries out fine de-sulfur defluorinate, and it is dense to obtain desulfurization defluorinate wet method by press filtration
Phosphorus.
By obtained desulfurization defluorinate phosphoric acid by wet process and 4 parts of compounded organic solvents, (tributyl phosphate and kerosene are according to volume ratio
4:1 ratio mixing) hybrid extraction, raffinate after extraction enters other production processes.
(2) 100 parts of the organic phase of extraction back loading phosphoric acid is washed for 1 part with wet cleaning phosphoric acid,diluted, the acid after washing
Into desulfurization defluorination process.
(3) 12 parts of organic phase after washing, is stripped for 1 part with deionized water, obtains wet cleaning phosphoric acid,diluted, gained
Wet cleaning phosphoric acid,diluted Fe contents are 7mg/kg, SO4 2-Content is 110mg/kg.
(4) 5 parts of organic phase after being stripped is that 1 part of 10% potassium hydroxide solution is washed with mass concentration, is washed
The organic phase after potassium dihydrogen phosphate containing organic impurities and washing after washing, the organic phase after washing enter (1) step into
Row hybrid extraction process.
(5) 1 part of wet cleaning phosphoric acid,diluted, mixing is added in 4 parts of the potassium dihydrogen phosphate containing organic impurities after washing
After be filtered to remove a large amount of solid organic impurities, it is 4-4.5 that filtrate, which adds potassium hydroxide and adjusts pH, concentration, crystallization, dry
Obtain potassium dihydrogen phosphate product, product purity 98%.
Embodiment 4
(1), according to weight, 1 part of P2O5Content be 42% (mass concentration) wet method concentrated phosphoric acid after sedimentation, filtering,
(tributyl phosphate and kerosene are according to volume ratio 4 with 3 parts of compound organic extractants for filtrate:1 ratio mixing) hybrid extraction obtains
The organic phase for loading phosphoric acid, the raffinate after extraction enter other production processes.
0.01 part of calcium oxide and 0.004 part of sodium hydroxide is added in the sour phase after 1 part of step (2) is washed, fully
After dissolving reaction, the extraction back loading phosphoric acid organic phase with 0.2 part is stirred, and 2h is stirred to react at 70 DEG C, is settled later
Split-phase returns to dissolving calcium oxide and sodium hydroxide after the sour phase press filtration after split-phase.Organic phase after split-phase enters step (2)
Washing.
(2), 10 parts of the organic phase after split-phase is washed for 1 part with Wet Phosphoric Acid Market, and mutually a part continues acid after washing
It returns to dissolving calcium oxide and sodium hydroxide, another part goes other production processes.
(3) 8 parts of organic phase after washing, is stripped for 1 part with deionized water, obtains wet cleaning phosphoric acid,diluted, gained is wet
It is 6mg/kg, SO that method, which purifies phosphoric acid,diluted Fe contents,4 2-Content is 35mg/kg.
(4) 3 parts of organic phase after being stripped is that 1 part of 5% potassium hydroxide solution carries out secondary washing with mass concentration, obtains
The organic phase after potassium dihydrogen phosphate containing organic impurities and secondary washing after washing, organic phase after secondary washing into
Enter (1) step and carries out hybrid extraction process.
(5) 1 part of wet cleaning phosphoric acid,diluted, mixing is added in 4 parts of the potassium dihydrogen phosphate containing organic impurities after washing
After be filtered to remove a large amount of solid organic impurities, it is 4-4.5 that filtrate, which adds potassium hydroxide and adjusts pH, concentration, crystallization, dry
Obtain potassium dihydrogen phosphate product, product purity 95%.
Embodiment 5
(1), according to weight, 1 part of P2O5Content be 43% (mass concentration) wet method concentrated phosphoric acid after sedimentation, filtering,
(tributyl phosphate and kerosene are according to volume ratio 4 with 5 parts of compound organic extractants for filtrate:1 ratio mixing) hybrid extraction obtains
The organic phase for loading phosphoric acid, the raffinate after extraction enter other production processes.
0.02 part of calcium oxide and 0.008 part of sodium hydroxide is added in the sour phase after 1 part of step (2) is washed, fully
After dissolving reaction, the extraction back loading phosphoric acid organic phase with 0.4 part is stirred, and 3h is stirred to react at 60 DEG C, is settled later
Split-phase returns to dissolving calcium oxide and sodium hydroxide after the sour phase press filtration after split-phase.Organic phase after split-phase enters step (2)
Washing.
(2), 20 parts of the organic phase after split-phase is washed for 1 part with Wet Phosphoric Acid Market, and mutually a part continues acid after washing
It returns to dissolving calcium oxide and sodium hydroxide, another part goes other production processes.
(3) 10 parts of organic phase after washing, is stripped for 1 part with deionized water, obtains wet cleaning phosphoric acid,diluted, gained
Wet cleaning phosphoric acid,diluted Fe contents are 5.6mg/kg, SO4 2-Content is 32.5mg/kg.
(4) 4 parts of organic phase after being stripped is that 1 part of 10% potassium hydroxide solution is washed with mass concentration, is washed
The organic phase after potassium dihydrogen phosphate containing organic impurities and washing after washing, the organic phase after washing enter (1) step into
Row hybrid extraction process.
(5) 1 part of wet cleaning phosphoric acid,diluted, mixing is added in 5 parts of the potassium dihydrogen phosphate containing organic impurities after washing
After be filtered to remove a large amount of solid organic impurities, it is 4-4.5 that filtrate, which adds potassium hydroxide and adjusts pH, concentration, crystallization, dry
Obtain potassium dihydrogen phosphate product, product purity 95.8%.
Embodiment 6
(1), according to weight, 1 part of P2O5Content be 4.5% (mass concentration) wet method concentrated phosphoric acid after sedimentation, filtering,
(tributyl phosphate and kerosene are according to volume ratio 4 with 3 parts of compound organic extractants for filtrate:1 ratio mixing) hybrid extraction obtains
The organic phase for loading phosphoric acid, the raffinate after extraction enter other production processes.
0.02 part of calcium oxide and 0.006 part of sodium hydroxide is added in the sour phase after 1 part of step (2) is washed, fully
After dissolving reaction, the extraction back loading phosphoric acid organic phase with 0.3 part is stirred, and 2h is stirred to react at 65 DEG C, is settled later
Split-phase returns to dissolving calcium oxide and sodium hydroxide after the sour phase press filtration after split-phase.Organic phase after split-phase enters step (2)
Washing.
(2), 30 parts of the organic phase after split-phase is washed for 1 part with Wet Phosphoric Acid Market, and mutually a part continues acid after washing
It returns to dissolving calcium oxide and sodium hydroxide, another part goes other production processes.
(3) 12 parts of organic phase after washing, is stripped for 1 part with deionized water, obtains wet cleaning phosphoric acid,diluted, gained
Wet cleaning phosphoric acid,diluted Fe contents are 5.6mg/kg, SO4 2-Content is 31.9mg/kg.
(4) 3 parts of organic phase after being stripped is that 1 part of 15% potassium hydroxide solution carries out secondary washing with mass concentration, obtains
The organic phase after potassium dihydrogen phosphate containing organic impurities and secondary washing after to washing, the organic phase after secondary washing
Hybrid extraction process is carried out into (1) step.
(5) 1 part of wet cleaning phosphoric acid,diluted, mixing is added in 4 parts of the potassium dihydrogen phosphate containing organic impurities after washing
After be filtered to remove a large amount of solid organic impurities, it is 4-4.5 that filtrate, which adds potassium hydroxide and adjusts pH, concentration, crystallization, dry
Obtain potassium dihydrogen phosphate product, product purity 95%.
Although an embodiment of the present invention has been shown and described, it will be understood by those skilled in the art that：Not
In the case of being detached from the principle of the present invention and objective a variety of change, modification, replacement and modification can be carried out to these embodiments,
The scope of the present invention is limited by claim and its equivalent.
Claims (9)
1. a kind of method of Purification of Wet process Phosphoric Acid by Solvent Extraction coproduction potassium dihydrogen phosphate, which is characterized in that including with following work
Skill step：
(1), phosphoric acid by wet process obtains desulfurization defluorinate phosphoric acid by wet process after desulfurization defluorination process sedimentation filtration, then with compound organic molten
The process that load organic phases are obtained by extraction in agent；
Or after phosphoric acid by wet process is directly over sedimentation, extracted using compounded organic solvent, in the organic phase for then loading phosphoric acid
Desulfurization defluorinating agent is added and carries out desulfurization defluorinate, then sedimentation, split-phase obtain load organic phases；
The compounded organic solvent is the mixture of tributyl phosphate and kerosene；
(2), the process that load organic phases are washed with wet cleaning phosphoric acid,diluted, the acid after washing are collected spare；
(3), the load organic phases after washing are stripped the process for obtaining wet cleaning phosphoric acid,diluted using deionized water；
(4), the organic phase after being stripped is washed using potassium hydroxide solution, the organic phase after being washed and cleaning solution, wherein washing
Extractant is used as in organic phase return to step (1) after washing；
(5), wet cleaning phosphoric acid,diluted is added in the cleaning solution in step (4), is filtered after mixing, removes solid organic impurities, then
Potassium hydroxide is added in filtrate and adjusts pH4-4.5, concentrates, crystallize, be dried to obtain potassium dihydrogen phosphate product.
2. the method for Purification of Wet process Phosphoric Acid by Solvent Extraction coproduction potassium dihydrogen phosphate according to claim 1, which is characterized in that
In step (1), the technique of desulfurization defluorinate is before extracting：According to parts by weight, 0.02-0.03 parts are added in a phosphoric acid by wet process
The thick desulfurization of calcium oxide, be separated by solid-liquid separation after sedimentation, add in the liquid phase 0.005 part -0.01 part barium carbonate and 0.002 part -1
The sodium hydroxide fine de-sulfur defluorinate of part, desulfurization defluorinate wet method concentrated phosphoric acid is obtained by press filtration.
3. the method for Purification of Wet process Phosphoric Acid by Solvent Extraction coproduction potassium dihydrogen phosphate according to claim 1, which is characterized in that
In step (1), the technique of desulfurization defluorinate is after extraction：0.01-0.02 parts are added in the acid after washing in a step (2)
Calcium oxide and 0.004-0.008 parts of sodium hydroxide, fully dissolving reaction after, with 0.2-0.4 part load phosphoric acid it is organic
It is mutually stirred and carries out desulfurization defluorination reaction, then settle split-phase, returned after the sour phase press filtration after split-phase and continue to dissolve calcium oxide
And sodium hydroxide, the organic phase after split-phase enter step (2) washing procedure.
4. according to the method for any one of the claim 1-3 Purification of Wet process Phosphoric Acid by Solvent Extraction coproduction potassium dihydrogen phosphates,
It is characterized in that, the technique of extraction is：It is added in every part of desulfurization defluorinate phosphoric acid by wet process or the phosphoric acid by wet process being directly over after sedimentation
2-5 parts of compounded organic solvents are extracted.
5. the method for Purification of Wet process Phosphoric Acid by Solvent Extraction coproduction potassium dihydrogen phosphate according to claim 4, it is characterised in that：
Per 10-100 parts of load organic phases with the 1 part of washing of wet cleaning phosphoric acid,diluted in step (2).
6. the method for Purification of Wet process Phosphoric Acid by Solvent Extraction coproduction potassium dihydrogen phosphate according to claim 5, it is characterised in that：
Load organic phases per 8-12 parts after washing are stripped using 1 part of deionized water.
7. the method for Purification of Wet process Phosphoric Acid by Solvent Extraction coproduction potassium dihydrogen phosphate according to claim 6, it is characterised in that：
In step (4), the organic phase per 3-5 parts after back extraction is washed using 1 part of potassium hydroxide solution.
8. the method for Purification of Wet process Phosphoric Acid by Solvent Extraction coproduction potassium dihydrogen phosphate according to claim 7, it is characterised in that：
The mass concentration of washing potassium hydroxide solution is 5%-15%.
9. the method for Purification of Wet process Phosphoric Acid by Solvent Extraction coproduction potassium dihydrogen phosphate according to claim 8, it is characterised in that：
In step (5), is filtered after 1 part of wet cleaning phosphoric acid,diluted mixing is added in every 4-6 parts of cleaning solution, remove solid organic impurities.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810725232.1A CN108609592A (en) | 2018-07-04 | 2018-07-04 | The method of Purification of Wet process Phosphoric Acid by Solvent Extraction coproduction potassium dihydrogen phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810725232.1A CN108609592A (en) | 2018-07-04 | 2018-07-04 | The method of Purification of Wet process Phosphoric Acid by Solvent Extraction coproduction potassium dihydrogen phosphate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108609592A true CN108609592A (en) | 2018-10-02 |
Family
ID=63666008
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810725232.1A Pending CN108609592A (en) | 2018-07-04 | 2018-07-04 | The method of Purification of Wet process Phosphoric Acid by Solvent Extraction coproduction potassium dihydrogen phosphate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108609592A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| WO2021251891A1 (en) * | 2020-06-12 | 2021-12-16 | Easymining Sweden Ab | Production of potassium phosphates |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1799996A (en) * | 2005-12-30 | 2006-07-12 | 云南省化工研究院 | Wet method phosphoric acid purification method |
| CN101177251A (en) * | 2007-10-26 | 2008-05-14 | 中化重庆涪陵化工有限公司 | Method for producing technical grade ribose phosphate, food grade ribose phosphate and industry ammonium diacid phosphate using wet-process ribose phosphate |
| CN101525130A (en) * | 2009-04-10 | 2009-09-09 | 武汉工程大学 | Technique for purifying and producing industrial phosphoric acid by wet-process phosphoric acid |
| CN101979311A (en) * | 2010-11-15 | 2011-02-23 | 中化重庆涪陵化工有限公司 | Method for producing industrial monopotassium phosphate and nitrogen, phosphorus and potassium compound fertilizer by using wet-process purified phosphoric acid as raw material through extraction |
-
2018
- 2018-07-04 CN CN201810725232.1A patent/CN108609592A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1799996A (en) * | 2005-12-30 | 2006-07-12 | 云南省化工研究院 | Wet method phosphoric acid purification method |
| CN101177251A (en) * | 2007-10-26 | 2008-05-14 | 中化重庆涪陵化工有限公司 | Method for producing technical grade ribose phosphate, food grade ribose phosphate and industry ammonium diacid phosphate using wet-process ribose phosphate |
| CN101525130A (en) * | 2009-04-10 | 2009-09-09 | 武汉工程大学 | Technique for purifying and producing industrial phosphoric acid by wet-process phosphoric acid |
| CN101979311A (en) * | 2010-11-15 | 2011-02-23 | 中化重庆涪陵化工有限公司 | Method for producing industrial monopotassium phosphate and nitrogen, phosphorus and potassium compound fertilizer by using wet-process purified phosphoric acid as raw material through extraction |
Non-Patent Citations (1)
| Title |
|---|
| 李淑兰等: "《化学与化工技术 科技学术论文集 2005》", 31 July 2005, 原子能出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021251891A1 (en) * | 2020-06-12 | 2021-12-16 | Easymining Sweden Ab | Production of potassium phosphates |
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100558633C (en) | The method for preparing PHOSPHORIC ACID TECH.GRADE, food grade phosphoric acid and industrial monoammonium phosphate with phosphoric acid by wet process | |
| CN1312030C (en) | Method for purifying wet-process phosphoric acid by crystallization | |
| CN114890450B (en) | Method for preparing scandium oxide | |
| CN102586612A (en) | Method for recovering vanadium and chromium from vanadium and chromium-containing slag | |
| CN106244828B (en) | A kind of impurity-removing method containing vanadium leachate | |
| CN101985694A (en) | Preparation method for recovering high-purity yttrium europium from fluorescent powder scrap | |
| CN110467229B (en) | Method for purifying nickel sulfate | |
| CN106435175A (en) | Method for preparing ammonium molybdate from molybdenum calcine by synergistic acid leaching method | |
| CN108609592A (en) | The method of Purification of Wet process Phosphoric Acid by Solvent Extraction coproduction potassium dihydrogen phosphate | |
| US20120315214A1 (en) | Method for preparing manganese sulfate monohydrate | |
| JP5867727B2 (en) | Separation method of rare earth elements | |
| JP6909826B2 (en) | A method for producing a vanadium compound, a method for producing an electrolytic solution for a redox flow battery, an apparatus for producing a vanadium compound, and an apparatus for producing an electrolytic solution for a redox flow battery. | |
| CN112875662B (en) | Method for purifying wet-process phosphoric acid by solvent extraction | |
| CN102887534A (en) | Method for recovering reagent level anhydrous sodium sulfate from raffinate obtained in process of extracting nickel from nickel sulfate solution | |
| CN110817819B (en) | Wet-process phosphoric acid purification system and preparation process thereof | |
| CN106586990B (en) | With the method for Wet-process Phosphoric Acid Production potassium dihydrogen phosphate | |
| CN109292807B (en) | Method for preparing 5N-grade strontium nitrate | |
| CN108622869A (en) | The method of Purification of Wet process Phosphoric Acid by Solvent Extraction | |
| CN116621134A (en) | Extraction crystallization process of wet phosphoric acid | |
| EP0432610B1 (en) | Concurrent production of citric acid and alkali citrates | |
| CN102925684A (en) | Method for preparing high-purity vanadium oxide | |
| CN105543475A (en) | Method for enriching and recovering rare earth from rare earth-containing phosphorite | |
| CN101928035B (en) | Method for removing calcium from copper sulphate solution | |
| CN110116997A (en) | A kind of method that wet phosphoric acid purifying removes iron | |
| CA1043535A (en) | Process for the preparation of purified phosphoric solutions from phosphoric acid in a wet way |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181002 |
|
| RJ01 | Rejection of invention patent application after publication |