CN102701167A - Method for producing industrial ammonium dihydrogen phosphate - Google Patents
Method for producing industrial ammonium dihydrogen phosphate Download PDFInfo
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- CN102701167A CN102701167A CN2012101946327A CN201210194632A CN102701167A CN 102701167 A CN102701167 A CN 102701167A CN 2012101946327 A CN2012101946327 A CN 2012101946327A CN 201210194632 A CN201210194632 A CN 201210194632A CN 102701167 A CN102701167 A CN 102701167A
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- phosphoric acid
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- acid
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Abstract
The invention discloses a method for producing industrial ammonium dihydrogen phosphate, which comprises the following steps: 1) adding a certain amount of phosphorite slurry into phosphoric acid by wet process, reacting and standing by for a period of time, and initially desulfurizing; 2) taking supernatant liquor, adding a certain amount of barium salt and sodium salt, thereby deeply desulfurizing and defluorinating; 3) introducing ammonia for neutralizing, and then filtering, thereby obtaining an ammonium acid phosphate solution containing few impurities; and 4) mixing the solution with phosphoric acid purified according to a solvent extraction method in proportion, adjusting neutralizing degree, concentrating and crystallizing, thereby obtaining the industrial ammonium dihydrogen phosphate. A chemical precipitation method is used for purifying the phosphoric acid by wet process produced by using medium/low-grade phosphorite; the purifying degree is not enough, so that the chemical precipitation method cannot be directly used for producing the industrial ammonium dihydrogen phosphate. Less solvent is added for purifying the phosphoric acid according to the solvent extraction method and then the concentrating and crystallizing are performed, thereby obtaining the ammonium dihydrogen phosphate which can reach II class standard in HG/T4133-2010. The production cost is lowered.
Description
Technical field
The invention belongs to technical field of chemical engineering, relate to the working method of PHOSPHORIC ACID TECH.GRADE ammonium dihydrogen.
Background technology
The production of industrial phosphoric acid ammonium dihydrogen all is to adopt thermal phosphoric acid technology for a long time.But the variation of As market; And the restriction of factor such as resource, environment, the energy; The phosphoric acid and the inorganic phosphate production technology that are the basis with the wet phosphoric acid purifying technology replace traditional thermal phosphoric acid and phosphate production technical development very fast, become the focus of Modern Phosphating worker hi-tech development.The operational path that with sulfuric acid is raw material is fundamental method in the Wet-process Phosphoric Acid Production; Phosphoric acid by wet process comes down to the nitration mixture of phosphoric acid, sulfuric acid and silicofluoric acid; Contain plurality of impurities (like calcium, magnesium, fluorine, iron, aluminium, sulfate radical plasma); It is multiple fertile generally to be used to produce phosphorus; The phosphate product that is used for process industry level, feed grade even food grade must be with wet phosphoric acid purifying to remove impurity wherein, and the wet phosphoric acid purifying technology mainly contains following several kinds at present: solvent extration, crystallization process, ion exchange method and electroosmose process, chemical precipitation method and method of enrichment.
Before my company in the Chinese patent 200710092904.1 of application a kind of method for preparing PHOSPHORIC ACID TECH.GRADE, food grade phosphoric acid and industrial monoammonium phosphate with phosphoric acid by wet process is disclosed; Be the solvent extration purification of wet process phosphoric acid; Chinese patent 200510019734.5 also discloses a kind of method of phosphoric acid by wet process of solvent extraction purification mid low grade phosphate rock production, and the diluted acid quality of solvent extration gained can compare favourably with thermal phosphoric acid, ability direct production industrial phosphoric acid ammonium dihydrogen; But; This method need add organic solvent, high volatility, inflammable, explosive, cost an arm and a leg, it is higher to be used for process industry level primary ammonium phosphate cost.
Chemical precipitation method phosphoric acid purification flow process is short, and cost is low, but the quality that purifies acid is not high, the requirement that does not reach the manufacture primary ammonium phosphate again.How can produce the industrial phosphoric acid ammonium dihydrogen that meets II class standard among the HG/T4133-2010, improve the added value of mid low grade phosphate rock, simultaneously the manufacturing cost new direction that becomes insider's research on the low side.
Summary of the invention
In order to solve the problems of the technologies described above; The object of the present invention is to provide and a kind ofly utilize phosphoric acid that the chemical precipitation method purification of wet process phosphoric acid for preparing gets and mix the method for preparing the industrial phosphoric acid ammonium dihydrogen, low cost of manufacture with the phosphoric acid that the solvent extration purification of wet process phosphoric acid for preparing gets.
The present invention seeks to realize like this: a kind of method of manufacture primary ammonium phosphate, accomplish according to following steps:
(1), under agitation, in phosphoric acid by wet process, add the phosphorus ore slurry it is carried out preliminary desulfurization, the add-on of described phosphorus ore slurry is SO in the phosphoric acid by wet process
4 2-Stoichiometric 110%-120%, reaction was left standstill 10-16 hour, got supernatant liquid, measured SO in the supernatant
4 2-Content, under agitation, in supernatant, add sweetening agent and defluorinating agent again, the amount of said sweetening agent is SO in the supernatant
4 2-Stoichiometric 100%-110%, the amount of said defluorinating agent is F in the phosphoric acid by wet process
-Stoichiometric 100%～110%, continue reaction 0.5-1h, stop to stir;
(2), above-mentioned solution is squeezed into neutralizing well, under condition of stirring, feed liquefied ammonia, regulate PH5.5-6.5, in obtaining and slip;
(3), with in above-mentioned and slip filter and obtain aqueous phosphate solution;
(4), aqueous phosphate solution is concentrated; Add the diluted acid that obtains behind the solvent extraction purification of wet process phosphoric acid simultaneously; The adjusting degree of neutralization is 1.0-1.1, when pulp density reaches 1.4-1.5, and crystallisation by cooling; Centrifugal then, drying obtains the industrial phosphoric acid ammonium dihydrogen, the P of the diluted acid that obtains behind the wherein said solvent extraction purification of wet process phosphoric acid
2O
5Content>=20%, Fe
2+≤10ppm, SO
4 2-≤300ppm, F
-≤400ppm.
Adopt technique scheme, carry out elementary desulfurization with the phosphorus ore slurry earlier, add barium carbonate generation barium sulfate precipitate again and carry out deep desulfuration.Add sodium hydroxide and generate the defluorinate of Sodium Silicofluoride 98min deposition.Its reaction mechanism is distinguished as follows:
5H
2SO
4+Ca
5F(PO
4)
3+10H
2O→5CaSO
4 -2H
2O↓+HF↑+3H
3PO
4
BaCO
3+H
2SO
4→BaSO
4↓+H
2O+CO
2↑
H
2SiF
6+2NaOH→Na
2SiF
6↓+2H
2O
After the deep desulfuration defluorinate, the impurity in the phosphoric acid solution is mainly Fe
3+, Al
3+, Mg
2+Deng positively charged ion.Feed liquefied ammonia then, regulate the pH value, impurity is separated out with depositions such as phosphoric acid salt, double salt, nonphosphates.The chemical reaction of major impurity generation during this time has:
Fe(H
2PO
4)
3+4NH
3·H
2O→FePO
4·2H
2O↓+2(NH
4)
2HPO
4+2H
2O
Al(H
2PO
4)
3+4NH
3·H
2O→AlPO
4·2H
2O↓+2(NH
4)
2HPO
4+2H
2O
Mg(H
2PO
4)
2+2NH
3·H
2O+2H
2O→MgPO
4·4H
2O↓+(NH
4)
2HPO
4
MgSO
4+2NH
3·H
2O+H
3PO
4+2H
2O→MgHPO
4·4H
2O↓+(NH
4)
2SO
4
The diluted acid P that obtains after the purification of mixed extractant solvent method then
2O
5>=20%, make qualified industrial phosphoric acid ammonium dihydrogen.The extracting and purifying phosphoric acid that adds is about 1: 3 with the ratio of chemical purification phosphoric acid～and 4 (concrete extracting and purifying phosphoric acid add-on is confirmed according to the slip degree of neutralization) this method improved the added value of the phosphoric acid by wet process that mid low grade phosphate rock produces greatly; Reduced production cost, the PHOSPHORIC ACID TECH.GRADE ammonium dihydrogen of the present invention's preparation meets II class standard among the HG/T 4133-2010.
Gained filter cake (phosphorous) can return the composting system in the step 3 in addition.Phosphor resource is fully used.
In order to reduce the consumption of barium carbonate, the preliminary desulfurization of step 1 must add enough phosphorus ore slurries and guarantee reaction, time of repose.
In order to reduce the loss of phosphorus in the olefin(e) acid purification, the pH value can not surpass the upper limit in the step 2.
In technique scheme, filter through the plate and frame filter with slip in described in the step (3).
In technique scheme, mainly contain primary ammonium phosphate and Secondary ammonium phosphate in the said aqueous phosphate solution.
In technique scheme: the concrete steps of said solvent extraction purification phosphoric acid by wet process are:
(a) phosphoric acid by wet process is removed solid substance with being pumped into pressure filter, the clear liquid that obtains gets into extraction tower top, and the extraction tower bottom adds the extraction agent of 3-9 times of volume of clear liquid simultaneously; Said extraction agent is tributyl phosphate, thinner, discoloring agent; Proportion relation is 2: 1: 0.00005, under 45-55 ℃, carries out hybrid extraction, forms organic phase and extracting phase; After organic phase gets into desulfurization defluorinate groove and adds ability neutralisation of sulphuric acid radical ion and the fluorion 1.0-1.1 abundant stirring reaction of sweetening agent, defluorinating agent and regenerator doubly; Overflow gets into clarifying tank and carries out sedimentation, layering, and the bottom slurry is discharged after pressure filter filters, and filtrating is returned clarifying tank;
(b) inlet gets into the washing tower supernatant liquid in the clarifying tank from the bottom; Enter the mouth from the washing tower middle and lower part again and add the purifying phosphoric acid of said supernatant liquid 5-15 times volume; With said supernatant liquid thorough mixing and layering; Wherein upper organic phase flows into washing organic phase groove from washing tower top, squeezes into back extraction tower middle and lower part inlet with pump then, with add de-salted water thorough mixing and the layering of 7 times of volumes of said upper organic phase from back extraction tower middle and upper part inlet simultaneously after extraction agent flow out from extraction tower top; After the interchanger heat exchange, recycle, the back extraction dilute phosphoric acid flows into the finished acid medial launder from the extraction tower bottom; With pump the back extraction dilute phosphoric acid is sent into smart desulfurizer and the abundant stirring reaction of sweetening agent barium carbonate that adds 1.05 times of ability neutralisation of sulphuric acid radical ions simultaneously at last; To get into medial launder temporary in overflow from smart desulfurizer top, and with pump sending into of its being obtained filtrating after vertical type full automatic pressure filter filters again is the diluted acid that obtains behind the solvent extraction purification of wet process phosphoric acid.
In technique scheme, said sweetening agent is barium carbonate or ground phosphate rock or both mixing, and said defluorinating agent is a soda ash, and said regenerator is a caustic soda.
Beneficial effect: utilize the phosphoric acid that the chemical precipitation method purification of wet process phosphoric acid for preparing gets and prepare phosphoric acid and mix the method for preparing the industrial phosphoric acid ammonium dihydrogen with the phosphoric acid that the solvent extration purification of wet process phosphoric acid for preparing gets; Improved the added value of the phosphoric acid by wet process of mid low grade phosphate rock production; Reduced production cost, the PHOSPHORIC ACID TECH.GRADE ammonium dihydrogen of the present invention's preparation meets II class standard among the HG/T 4133-2010.
Embodiment
Below in conjunction with embodiment the present invention is done further explanation:
According to Chinese patent 200710092904.1 disclosed solvent extration purification of wet process phosphoric acid, obtain the diluted acid that obtains behind the solvent extraction purification of wet process phosphoric acid, its concrete steps are: (a) phosphoric acid by wet process is removed solid substance with being pumped into pressure filter; The clear liquid that obtains gets into extraction tower top; The extraction tower bottom adds the extraction agent of 3-9 times of volume of clear liquid simultaneously, and said extraction agent is tributyl phosphate, thinner, discoloring agent, and proportion relation is 2: 1: 0.00005; Under 45-55 ℃, carry out hybrid extraction; Form organic phase and extracting phase, after organic phase got into desulfurization defluorinate groove and adds ability neutralisation of sulphuric acid radical ion and the fluorion 1.0-1.1 abundant stirring reaction of sweetening agent, defluorinating agent and regenerator doubly, overflow got into clarifying tank and carries out sedimentation, layering; The bottom slurry is discharged after pressure filter filters, and filtrating is returned clarifying tank;
(b) inlet gets into the washing tower supernatant liquid in the clarifying tank from the bottom; Enter the mouth from the washing tower middle and lower part again and add the purifying phosphoric acid of said supernatant liquid 5-15 times volume; With said supernatant liquid thorough mixing and layering; Wherein upper organic phase flows into washing organic phase groove from washing tower top, squeezes into back extraction tower middle and lower part inlet with pump then, with add de-salted water thorough mixing and the layering of 7 times of volumes of said upper organic phase from back extraction tower middle and upper part inlet simultaneously after extraction agent flow out from extraction tower top; After the interchanger heat exchange, recycle, the back extraction dilute phosphoric acid flows into the finished acid medial launder from the extraction tower bottom; With pump the back extraction dilute phosphoric acid is sent into smart desulfurizer and the abundant stirring reaction of sweetening agent barium carbonate that adds 1.05 times of ability neutralisation of sulphuric acid radical ions simultaneously at last; To get into medial launder temporary in overflow from smart desulfurizer top, and with pump sending into of its being obtained filtrating after vertical type full automatic pressure filter filters again is the diluted acid that obtains behind the solvent extraction purification of wet process phosphoric acid.Said sweetening agent is barium carbonate or ground phosphate rock or both mixing, and said defluorinating agent is a soda ash, and said regenerator is a caustic soda.This method is open in Chinese patent 200710092904.1, it is not done at this and gives unnecessary details.The diluted acid that obtains behind certain solvent extraction purification of wet process phosphoric acid of the present invention also can not adopt disclosed method in the above-mentioned patent, as long as can satisfy the P of diluted acid
2O
5Content>=20%, Fe
2+≤10ppm, SO
4 2-≤300ppm, F
-The solvent extraction acid of≤400ppm all can be used for the present invention.
Embodiment 1
(1) gets phosphoric acid by wet process (P
2O
5Content is 20.2%, SO
4 2-Content is 2.5%, H
2SiF
6Content is 1.3%, Fe
2+Content is 0.25%) 70 tons, stir and add phosphorus ore slurry (P down
2O
5Content is 28%, water cut 30%) 4600 kilograms (be SO
4 2-Stoichiometric 117%, promptly phosphorus ore starches excessive 17%), reaction was left standstill 14 hours.Get supernatant liquid, measure SO in the supernatant once more
4 2-Content is 1.2%, and stirring down then, the adding barium carbonate (is SO for 1800 kilograms
4 2--Stoichiometric 106%, promptly barium carbonate excessive 6%), sodium hydroxide (is H for 505 kilograms
2SiF
6Stoichiometric 100%), reaction is 0.5 hour.
(2) above-mentioned solution is squeezed into neutralizing well, add liquefied ammonia neutralization, control PH is 5.5-6.5, in obtaining and slip.
(3) filter with the plate and frame filter with slip among the general, obtain ammonium phosphate solution (P
2O
5Content is 17.13%, SO
4 2-Content is 0.6%, F
-Content is 0.03%, Fe
2+Content is 6ppm).
(4) filtrating is squeezed into interchanger, and add the diluted acid that obtains behind the above-mentioned solvent extraction purification of wet process phosphoric acid, regulating degree of neutralization is 1.05.When pulp density is 1.45, put into the crystallisation by cooling groove, crystallisation by cooling, centrifugal, drying just obtain product (N+P
2O
5Content>=72%).Quality product satisfies HG/T 4133-2010II class standard.
Embodiment 2
Get phosphoric acid by wet process (P
2O
5Content is 20.0%, SO
4 2-Content is 2.7%, H
2SiF
6Content is 1.4%, Fe
2+Content is 0.22%) 70 tons, add phosphorus ore slurry (P
2O
5Content is 28%, water cut 30%) 5137 kilograms (be SO
4 2-Stoichiometric 120%, promptly phosphorus ore starches excessive 20%), reaction was left standstill 10 hours.Get supernatant liquid, measure phosphoric acid SO once more
4 2-Content is 1.2%, adds 1900 kilograms of barium carbonates then and (is SO
4 2--Stoichiometric 110%, promptly barium carbonate excessive 10%), sodium hydroxide (is H for 598 kilograms
2SiF
6Stoichiometric 110%, promptly sodium hydroxide excessive 10%).Reacted 1 hour.
(2) above-mentioned solution is squeezed into neutralizing well, feed the liquefied ammonia neutralization, control PH is 5.5-6.5, in obtaining and slip.
(3) filter with the plate and frame filter with slip among the general, obtain ammonium phosphate solution (P
2O
5Content is 17.84%, SO
4 2-Content is 0.7%, F
-Content is 0.03%, Fe
2+Content is 4ppm).
(4) filtrating is squeezed into interchanger, and add extracting and purifying acid, regulating degree of neutralization is 1.1.When pulp density is 1.5, put into the crystallisation by cooling groove, crystallisation by cooling, centrifugal, drying just obtain product (N+P
2O
5Content>=72%).Quality product satisfies HG/T 4133-2010II class standard.
Embodiment 3: phosphoric acid by wet process (P is got in (1)
2O
5Content is 20.2%, SO
4 2-Content is 2.5%, H
2SiF
6Content is 1.3%, Fe
2+Content is 0.25%) 70 tons, stir and add phosphorus ore slurry (P down
2O
5Content is 28%, water cut 30%) 4324 kilograms (be SO
4 2-Stoichiometric 110%, promptly phosphorus ore starches excessive 10%), reaction was left standstill 16 hours.Get supernatant liquid, measure SO in the supernatant once more
4 2-Content is 1.2%, and stirring down then, the adding barium carbonate (is SO for 1700 kilograms
4 2--Stoichiometric 100%), sodium hydroxide (is H for 505 kilograms
2SiF
6Stoichiometric 100%), reaction is 0.6 hour.
(2) above-mentioned solution is squeezed into neutralizing well, add liquefied ammonia neutralization, control PH is 5.5-6.5, in obtaining and slip.
(3) filter with the plate and frame filter with slip among the general, obtain ammonium phosphate solution (P
2O
5Content is 17.13%, SO
4 2-Content is 0.6%, F
-Content is 0.03%, Fe
2+Content is 6ppm).
(4) filtrating is squeezed into interchanger, and add the diluted acid that obtains behind the above-mentioned solvent extraction purification of wet process phosphoric acid, regulating degree of neutralization is 1.0.When pulp density is 1.4, put into the crystallisation by cooling groove, crystallisation by cooling, centrifugal, drying just obtain product (N+P
2O
5Content>=72%).Quality product satisfies HG/T 4133-2010II class standard.
Claims (5)
1. the method for a manufacture primary ammonium phosphate is characterized in that: accomplish according to following steps:
(1), under agitation, in phosphoric acid by wet process, add the phosphorus ore slurry it is carried out preliminary desulfurization, the add-on of described phosphorus ore slurry is SO in the phosphoric acid by wet process
4 2-Stoichiometric 110%-120%, reaction was left standstill 10-16 hour, got supernatant liquid, measured SO in the supernatant
4 2-Content, under agitation, in supernatant, add sweetening agent and defluorinating agent again, the amount of said sweetening agent is SO in the supernatant
4 2-Stoichiometric 100%-110%, the amount of said defluorinating agent is F in the phosphoric acid by wet process
-Stoichiometric 100%～110%, continue reaction 0.5-1h, stop to stir;
(2), above-mentioned solution is squeezed into neutralizing well, under condition of stirring, feed liquefied ammonia, regulate PH5.5-6.5, in obtaining and slip;
(3), with in above-mentioned and slip filter and obtain aqueous phosphate solution;
(4), aqueous phosphate solution is concentrated; Add the diluted acid that obtains behind the solvent extraction purification of wet process phosphoric acid simultaneously; The adjusting degree of neutralization is 1.0-1.1, when pulp density reaches 1.4-1.5, and crystallisation by cooling; Centrifugal then, drying obtains the industrial phosphoric acid ammonium dihydrogen, the P of the diluted acid that obtains behind the wherein said solvent extraction purification of wet process phosphoric acid
2O
5Content>=20%, Fe
2+≤10ppm, SO
4 2-≤300ppm, F
-≤400ppm.
2. according to the method for the said manufacture primary ammonium phosphate of claim 1, it is characterized in that: filter through the plate and frame filter with slip in described in the step (3).
3. according to the method for the said manufacture primary ammonium phosphate of claim 1, it is characterized in that: mainly contain primary ammonium phosphate and Secondary ammonium phosphate in the said aqueous phosphate solution.
4. according to the method for the said manufacture primary ammonium phosphate of claim 1, it is characterized in that: the concrete steps of said solvent extraction purification phosphoric acid by wet process are:
(a) phosphoric acid by wet process is removed solid substance with being pumped into pressure filter, the clear liquid that obtains gets into extraction tower top, and the extraction tower bottom adds the extraction agent of 3-9 times of volume of clear liquid simultaneously; Said extraction agent is tributyl phosphate, thinner, discoloring agent; Proportion relation is 2: 1: 0.00005, under 45-55 ℃, carries out hybrid extraction, forms organic phase and extracting phase; After organic phase gets into desulfurization defluorinate groove and adds ability neutralisation of sulphuric acid radical ion and the fluorion 1.0-1.1 abundant stirring reaction of sweetening agent, defluorinating agent and regenerator doubly; Overflow gets into clarifying tank and carries out sedimentation, layering, and the bottom slurry is discharged after pressure filter filters, and filtrating is returned clarifying tank;
(b) inlet gets into the washing tower supernatant liquid in the clarifying tank from the bottom; Enter the mouth from the washing tower middle and lower part again and add the purifying phosphoric acid of said supernatant liquid 5-15 times volume; With said supernatant liquid thorough mixing and layering, wherein upper organic phase flows into washing organic phase groove from washing tower top, squeezes into back extraction tower middle and lower part inlet with pump then; After adding the de-salted water thorough mixing and layering of 7 times of volumes of said upper organic phase from back extraction tower middle and upper part inlet simultaneously; Extraction agent flows out from extraction tower top, after the interchanger heat exchange, recycles, and the back extraction dilute phosphoric acid flows into the finished acid medial launder from the extraction tower bottom; With pump the back extraction dilute phosphoric acid is sent into smart desulfurizer and the abundant stirring reaction of sweetening agent barium carbonate that adds 1.05 times of ability neutralisation of sulphuric acid radical ions simultaneously at last; To get into medial launder temporary in overflow from smart desulfurizer top, and with pump sending into of its being obtained filtrating after vertical type full automatic pressure filter filters again is the diluted acid that obtains behind the solvent extraction purification of wet process phosphoric acid.
5. according to the method for the said manufacture primary ammonium phosphate of claim 4, it is characterized in that: said sweetening agent is barium carbonate or ground phosphate rock or both mixing, and said defluorinating agent is a soda ash, and said regenerator is a caustic soda.
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|---|---|---|---|
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|---|---|---|---|
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Cited By (9)
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| CN103641093A (en) * | 2013-11-02 | 2014-03-19 | 耿兆翔 | Phosphoric acid desulphurization or/and defluorination method for ammonium biphosphate industrial production |
| CN105776169A (en) * | 2016-04-05 | 2016-07-20 | 瓮福（集团）有限责任公司 | Method for washing phosphoric acid loaded organic solvent with compound washing agent |
| CN106629644A (en) * | 2017-01-14 | 2017-05-10 | 湖南省正源储能材料与器件研究所 | Method for producing industrial first-stage and battery-stage monoammonium phosphate by using fertilizer-stage monoammonium phosphate |
| CN109231182A (en) * | 2018-08-28 | 2019-01-18 | 深圳市德方纳米科技股份有限公司 | The method of ammonium dihydrogen phosphate, the preparation method of iron manganese phosphate for lithium and lithium iron phosphate positive material are prepared by phosphorus ore |
| CN110921642A (en) * | 2019-12-18 | 2020-03-27 | 瓮福（集团）有限责任公司 | Method and device for treating phosphoric acid slurry by wet process |
| CN111777052A (en) * | 2020-07-24 | 2020-10-16 | 瓮福（集团）有限责任公司 | Fine desulfurization method for phosphoric acid |
| CN113307243A (en) * | 2021-07-08 | 2021-08-27 | 河南佰利新能源材料有限公司 | Method for preparing iron phosphate by recycling mother liquor |
| CN113860277A (en) * | 2021-11-01 | 2021-12-31 | 瓮福（集团）有限责任公司 | Dihydrate wet process phosphoric acid production technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103641093A (en) * | 2013-11-02 | 2014-03-19 | 耿兆翔 | Phosphoric acid desulphurization or/and defluorination method for ammonium biphosphate industrial production |
| CN105776169A (en) * | 2016-04-05 | 2016-07-20 | 瓮福（集团）有限责任公司 | Method for washing phosphoric acid loaded organic solvent with compound washing agent |
| CN106629644A (en) * | 2017-01-14 | 2017-05-10 | 湖南省正源储能材料与器件研究所 | Method for producing industrial first-stage and battery-stage monoammonium phosphate by using fertilizer-stage monoammonium phosphate |
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| CN109231182A (en) * | 2018-08-28 | 2019-01-18 | 深圳市德方纳米科技股份有限公司 | The method of ammonium dihydrogen phosphate, the preparation method of iron manganese phosphate for lithium and lithium iron phosphate positive material are prepared by phosphorus ore |
| CN110921642B (en) * | 2019-12-18 | 2023-12-26 | 瓮福（集团）有限责任公司 | Wet-process phosphoric acid slurry treatment method and device |
| CN110921642A (en) * | 2019-12-18 | 2020-03-27 | 瓮福（集团）有限责任公司 | Method and device for treating phosphoric acid slurry by wet process |
| CN111777052A (en) * | 2020-07-24 | 2020-10-16 | 瓮福（集团）有限责任公司 | Fine desulfurization method for phosphoric acid |
| CN111777052B (en) * | 2020-07-24 | 2023-04-25 | 瓮福（集团）有限责任公司 | Fine desulfurization method for phosphoric acid |
| CN113307243B (en) * | 2021-07-08 | 2023-01-24 | 河南佰利新能源材料有限公司 | Method for preparing iron phosphate by recycling mother liquor |
| CN113307243A (en) * | 2021-07-08 | 2021-08-27 | 河南佰利新能源材料有限公司 | Method for preparing iron phosphate by recycling mother liquor |
| CN113860277A (en) * | 2021-11-01 | 2021-12-31 | 瓮福（集团）有限责任公司 | Dihydrate wet process phosphoric acid production technology |
| CN114735668A (en) * | 2022-04-01 | 2022-07-12 | 贵州开磷集团股份有限公司 | Production method of fire-fighting-grade monoammonium phosphate |
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Application publication date: 20121003 |