CN106586990B - With the method for Wet-process Phosphoric Acid Production potassium dihydrogen phosphate - Google Patents

With the method for Wet-process Phosphoric Acid Production potassium dihydrogen phosphate Download PDF

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CN106586990B
CN106586990B CN201610988560.1A CN201610988560A CN106586990B CN 106586990 B CN106586990 B CN 106586990B CN 201610988560 A CN201610988560 A CN 201610988560A CN 106586990 B CN106586990 B CN 106586990B
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phosphoric acid
dihydrogen phosphate
potassium dihydrogen
potassium
wet
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CN106586990A (en
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李兵
韦莎
张治平
郑义文
江涛
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Yangtze Normal University
Sinochem Fuling Chongqing Chemical Industry Co Ltd
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Yangtze Normal University
Sinochem Fuling Chongqing Chemical Industry Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/26Phosphates
    • C01B25/30Alkali metal phosphates
    • C01B25/301Preparation from liquid orthophosphoric acid or from an acid solution or suspension of orthophosphates
    • C01B25/303Preparation from liquid orthophosphoric acid or from an acid solution or suspension of orthophosphates with elimination of impurities
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

Abstract

The invention discloses a kind of methods with Wet-process Phosphoric Acid Production potassium dihydrogen phosphate, phosphate ore pulp and barium carbonate are sequentially added into phosphoric acid by wet process, the concentration of sulfate ion in phosphoric acid is set to be down to 0.5g/L, it is fine de-sulfur phosphoric acid,diluted that supernatant liquor acid is taken after standing sedimentation, above-mentioned fine de-sulfur phosphoric acid,diluted is extracted according to the composite extractant that arbitrary proportion mixes with octylame and octanol, split-phase is stood, the organic phase for coupling phosphoric acid is extract liquor, and remaining phosphoric acid is raffinate;Potassium chloride is added into above-mentioned extract liquor to be reacted, split-phase is stood, lower layer is the thick solution of potassium dihydrogen phosphate, upper layer is the organic phase rich in hydrochloric acid and a small amount of phosphoric acid and potassium chloride;After the thick solution filtering of potassium dihydrogen phosphate, it is about 6 that potassium hydroxide is added into filtrate and adjusts pH value of solution, and impurity is filtered off after standing sedimentation and obtains potassium dihydrogen phosphate essence solution;Into above-mentioned potassium dihydrogen phosphate essence solution plus purifying phosphoric acid adjusts pH as 4-5, and acquired solution condensing crystallizing filtration drying obtains potassium dihydrogen phosphate product.Process flow is simple, at low cost.

Description

With the method for Wet-process Phosphoric Acid Production potassium dihydrogen phosphate
Technical field
The present invention relates to a kind of methods with Wet-process Phosphoric Acid Production potassium dihydrogen phosphate, belong to solvent extraction production di(2-ethylhexyl)phosphate Hydrogen potassium technique.
Background technique
Potassium dihydrogen phosphate has extensive purposes in industrial and agricultural production.Industrially it is used as buffer, hardening agent, flavoring agent 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.
Currently, the production method of potassium dihydrogen phosphate mainly has neutralisation, double decomposition, solvent extraction etc..The country uses The process flow of solvent extraction production potassium dihydrogen phosphate are as follows: phosphoric acid by wet process desulfurization, defluorinate, then with organic solvent extracting and purifying, The extraction acid sludge that purification process generates is used to produce fertilizer;Potassium chloride solution is added in purified phosphoric acid and organic solvent carries out Extraction and separation, aqueous solution be after the solution of potassium dihydrogen phosphate, concentrate drying potassium dihydrogen phosphate product, rich in the organic of chloride ion Communicate ammonia back extraction after organic phase can be used as extractant be recycled, aqueous solution be concentrated and dried to obtain N P and K ternary compound fertilizer.It should Method is needed using two kinds of organic solvents, and there are two the extraction process in stage, operation cost is high.
In addition have after being purified acid using phosphoric acid by wet process solvent extraction, neutralize to obtain ammonium dihydrogen phosphate with ammonia molten Liquid adds potassium chloride later and carries out metathesis reaction.The potassium dihydrogen phosphate product purity that the method obtains is not very well, to need two Secondary crystallization.
It can be seen that the prior art all exists, removal of impurities is not thorough, mother liquor cannot be utilized rationally, extractant consumption is more, So that phosphrus reagent is relatively low, the production cost increases, these are all this field urgent problems to be solved.
Summary of the invention
For existing problem, the purpose of the present invention is to provide a kind of sides with Wet-process Phosphoric Acid Production potassium dihydrogen phosphate Method, production cost be low, the removal of simple process, impurity is thorough.
To achieve the goals above, the technical scheme is that such: a kind of to use Wet-process Phosphoric Acid Production biphosphate The method of potassium, includes the following steps:
A, phosphate ore pulp reaction is added into phosphoric acid by wet process, the concentration of sulfate ion in phosphoric acid is made to be down to 8g/L hereinafter, quiet Take supernatant liquor sour after setting sedimentation;
B, into supernatant liquor acid, the reaction was continued for addition barium carbonate, and the concentration of sulfate ion in phosphoric acid is made to be down to 0.5g/ L, it is fine de-sulfur phosphoric acid,diluted that supernatant liquor acid is taken after standing sedimentation;
C, above-mentioned fine de-sulfur phosphoric acid,diluted is extracted according to the composite extractant that arbitrary proportion mixes with octylame and octanol, it is quiet Split-phase is set, the organic phase for coupling phosphoric acid is extract liquor, and remaining phosphoric acid is raffinate;
D, in Xiang Shangshu extract liquor be added potassium chloride reacted, stand split-phase, lower layer 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;
E, in step d after the thick solution filtering of potassium dihydrogen phosphate, it is about 6 that potassium hydroxide is added into filtrate and adjusts pH value of solution, Impurity is filtered off after standing sedimentation obtains potassium dihydrogen phosphate essence solution;
In f: Xiang Shangshu potassium dihydrogen phosphate essence solution plus purifying phosphoric acid adjusting pH is 4-5, acquired solution condensing crystallizing, mistake It filters, be dried to obtain potassium dihydrogen phosphate product, filtrate is potassium dihydrogen phosphate mother liquor.
Using the above scheme, sulfate radical can be played the role of by increasing step a and b, and sulfate radical foreign matter removal is more Thoroughly, step c is used as extractant using octylame and octanol double solvents, octylame be it is alkaline, capable of playing fluorine removal and chlorine, (fluorine is in alkali Property under the conditions of can and cation complex, generate the precipitating such as fluosilicic acid iron aluminium), reduce defluorinate process, reduce cost.Using compound Extractant elder generation enrichment acid, removes hydrochloric acid again after mixing later with potassium chloride, only extract once, reduce production cost, secondly, The quality of raffinate less, alleviates subsequent ammonium phosphate production system load compared with ortho acid variation.
In above scheme: composite extractant and fine de-sulfur phosphoric acid,diluted is comparably 1:2-1 in step c;Between 4, reaction temperature Degree is 50-70 DEG C, reaction time 30-40min.
In above scheme, in the composite extractant, the volume ratio of octylame and octanol is 6:4-8:1.It is able to satisfy enough Octylame participates in reaction.
In above scheme, potassium chloride and P in extract liquor in step d2O5Molar ratio between 1.03-1.05, reaction temperature Degree is 50-70 DEG C, reaction time 20-40min.
In above 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 compound fertilizer.The quality of raffinate less, alleviates subsequent ammonium phosphate production system load compared with ortho acid variation.
In above scheme, ammonium hydroxide is added in the organic phase into step d rich in hydrochloric acid and a small amount of phosphoric acid and potassium chloride and adjusts PH is 7-8, and reaction temperature is 50-70 DEG C, reaction time 20-40min, stands split-phase, lower liquid is concentrated to give N P and K three Component composite fertilizer byproduct;Upper layer is extractant phase, is recycled as the extractant in step c.
In above scheme: carrying out the reaction of extraction split-phase in the potassium dihydrogen phosphate mother liquor return step d in step f.
The beneficial effects of the present invention are: 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, need to only extract once, reduce the use of phosphoric acid purification extractant, reduce and be produced into This;And raffinate quality less, alleviates the load of subsequent ammonium phosphate production system compared with ortho acid variation;Again, using compound extraction When agent being taken to extract, fluorine ion is also separated with precipitation form from the solution of potassium dihydrogen phosphate, reduces defluorinate process, further Reduce production cost.Obtained good product quality.
Specific embodiment
The present invention will be further described combined with specific embodiments below:
Embodiment 1
A method of with Wet-process Phosphoric Acid Production potassium dihydrogen phosphate, complete in accordance with the following steps:
A, the phosphate ore pulp that 50kg moisture content is 35% is added into 1000kg phosphoric acid by wet process, is stirred to react at 80 DEG C 2h makes the concentration of sulfate ion in phosphoric acid be down to 8g/L hereinafter, taking supernatant liquor sour after standing sedimentation.
B, 13.8kg barium carbonate is added into 800kg supernatant liquor acid, is down to the concentration of sulfate ion in phosphoric acid 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 of composite extractant extraction mixed with octylame and octanol according to the ratio of volume ratio 4:1 is dilute The volume ratio of phosphoric acid, composite extractant and fine de-sulfur phosphoric acid,diluted is 1:2, and reaction temperature is 50 DEG C, reaction time 30min, quiet Setting the split-phase time is 20-30min.The organic phase for coupling phosphoric acid is extract liquor, 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 compound fertilizer.
D, Klorvess Liquid is added in Xiang Shangshu extract liquor to be reacted, the volume ratio of extract liquor and Klorvess Liquid is 2: 1, P in potassium chloride and extract liquor2O5Molar ratio be 1.03, reaction temperature be 50 DEG C, reaction time 40min, stand split-phase when Between be 20-30min lower layer be the thick solution of potassium dihydrogen phosphate, upper layer be the organic phase rich in hydrochloric acid and a small amount of phosphoric acid and potassium chloride. It is 7-8 that ammonium hydroxide is added in organic phase rich in hydrochloric acid and a small amount of phosphoric acid and potassium chloride and adjusts pH, and reaction temperature is 50-70 DEG C, instead It is 20-40min between seasonable, stands split-phase, lower liquid is concentrated to give N P and K ternary compound fertilizer byproduct;Upper layer is extractant Phase is recycled as the extractant in step c.
E, in step d after the thick solution filtering of potassium dihydrogen phosphate, it is about 6 that potassium hydroxide is added into filtrate and adjusts pH value of solution, Impurity is filtered off after standing sedimentation obtains potassium dihydrogen phosphate essence solution.
In f: Xiang Shangshu potassium dihydrogen phosphate essence solution plus purifying phosphoric acid adjusting pH is 4, and acquired solution condensing crystallizing, which is crossed, to be 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 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 method of with Wet-process Phosphoric Acid Production potassium dihydrogen phosphate, complete in accordance with the following steps:
A, the phosphate ore pulp that 50kg moisture content is 35% is added into 1000kg phosphoric acid by wet process, is stirred to react at 80 DEG C 2h makes the concentration of sulfate ion in phosphoric acid be down to 8g/L hereinafter, taking supernatant liquor sour after standing sedimentation.
B, 13.8kg barium carbonate is added into 800kg supernatant liquor acid, is down to the concentration of sulfate ion in phosphoric acid 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 of composite extractant extraction mixed with octylame and octanol according to the ratio of volume ratio 8:1 is dilute The volume ratio of phosphoric acid, composite extractant and fine de-sulfur phosphoric acid,diluted is 1:4, and reaction temperature is 70 DEG C, reaction time 40min, quiet Setting the split-phase time is 20-30min.The organic phase for coupling phosphoric acid is extract liquor, 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 compound fertilizer.
D, Klorvess Liquid is added in Xiang Shangshu extract liquor to be reacted, the volume ratio of extract liquor and Klorvess Liquid is 2: 1, P in potassium chloride and extract liquor2O5Molar ratio be 1.05, reaction temperature be 70 DEG C, reaction time 20min, stand split-phase when Between be 20-30min lower layer be the thick solution of potassium dihydrogen phosphate, upper layer be the organic phase rich in hydrochloric acid and a small amount of phosphoric acid and potassium chloride. It is 7-8 that ammonium hydroxide is added in organic phase rich in hydrochloric acid and a small amount of phosphoric acid and potassium chloride and adjusts pH, and reaction temperature is 50-70 DEG C, instead It is 20-40min between seasonable, stands split-phase, lower liquid is concentrated to give N P and K ternary compound fertilizer byproduct;Upper layer is extractant Phase is recycled as the extractant in step c.
E, in step d after the thick solution filtering of potassium dihydrogen phosphate, it is about 6 that potassium hydroxide is added into filtrate and adjusts pH value of solution, Impurity is filtered off after standing sedimentation obtains potassium dihydrogen phosphate essence solution.
In f: Xiang Shangshu potassium dihydrogen phosphate essence solution plus purifying phosphoric acid adjusting pH is 5, and acquired solution condensing crystallizing, which is crossed, to be 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 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 method of with Wet-process Phosphoric Acid Production potassium dihydrogen phosphate, complete in accordance with the following steps:
A, the phosphate ore pulp that 50kg moisture content is 35% is added into 1000kg phosphoric acid by wet process, is stirred to react at 80 DEG C 2h makes the concentration of sulfate ion in phosphoric acid be down to 8g/L hereinafter, taking supernatant liquor sour after standing sedimentation.
B, 13.8kg barium carbonate is added into 800kg supernatant liquor acid, is down to the concentration of sulfate ion in phosphoric acid 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 of composite extractant extraction mixed with octylame and octanol according to the ratio of volume ratio 6:4 is dilute The volume ratio of phosphoric acid, composite extractant and fine de-sulfur phosphoric acid,diluted is 1:3, and reaction temperature is 60 DEG C, reaction time 30min, quiet Setting the split-phase time is 20-30min.The organic phase for coupling phosphoric acid is extract liquor, 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 compound fertilizer.
D, Klorvess Liquid is added in Xiang Shangshu extract liquor to be reacted, the volume ratio of extract liquor and Klorvess Liquid is 2: 1, P in potassium chloride and extract liquor2O5Molar ratio be 1.04, reaction temperature be 60 DEG C, reaction time 30min, stand split-phase when Between be 20-30min lower layer be the thick solution of potassium dihydrogen phosphate, upper layer be the organic phase rich in hydrochloric acid and a small amount of phosphoric acid and potassium chloride. It is 7-8 that ammonium hydroxide is added in organic phase rich in hydrochloric acid and a small amount of phosphoric acid and potassium chloride and adjusts pH, and reaction temperature is 50-70 DEG C, instead It is 20-40min between seasonable, stands split-phase, lower liquid is concentrated to give N P and K ternary compound fertilizer byproduct;Upper layer is extractant Phase is recycled as the extractant in step c.
E, in step d after the thick solution filtering of potassium dihydrogen phosphate, it is about 6 that potassium hydroxide is added into filtrate and adjusts pH value of solution, Impurity is filtered off after standing sedimentation obtains potassium dihydrogen phosphate essence solution.
In f: Xiang Shangshu potassium dihydrogen phosphate essence solution plus purifying phosphoric acid adjusting pH is 4.5, the filtering of acquired solution condensing crystallizing It is dried to obtain potassium dihydrogen phosphate product, filtrate is potassium dihydrogen phosphate mother liquor.It is extracted in potassium dihydrogen phosphate mother liquor return 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 should be understood that those skilled in the art are without creativeness Labour, which according to the present invention can conceive, makes many modifications and variations.In short, all technician in the art are according to this The design of invention passes through the available technical side of logical analysis, reasoning, or a limited experiment on the basis of existing technology Case, all should be within the scope of protection determined by the claims.

Claims (5)

1. a kind of method with Wet-process Phosphoric Acid Production potassium dihydrogen phosphate, includes the following steps:
A, phosphate ore pulp reaction is added into phosphoric acid by wet process, so that the concentration of sulfate ion in phosphoric acid is down to 8g/L and sinks hereinafter, standing Take supernatant liquor sour after drop;
B, into supernatant liquor acid, the reaction was continued for addition barium carbonate, and the concentration of sulfate ion in phosphoric acid is made to be down to 0.5g/L, quiet Take supernatant liquor acid for fine de-sulfur phosphoric acid,diluted after setting sedimentation;
C, above-mentioned fine de-sulfur phosphoric acid,diluted is extracted according to the composite extractant that arbitrary proportion mixes with octylame and octanol, stands and divides Phase, the organic phase for coupling phosphoric acid is extract liquor, and remaining phosphoric acid is raffinate;Wherein, composite extractant and fine de-sulfur phosphoric acid,diluted It is comparably between 1:2-1:4, reaction temperature is 50-70 DEG C, reaction time 30-40min;In the composite extractant, octylame Volume ratio with octanol is 6:4-8:1;
D, potassium chloride is added in Xiang Shangshu extract liquor to be reacted, stands split-phase, lower layer is the thick solution of potassium dihydrogen phosphate, upper layer is Organic phase rich in hydrochloric acid and a small amount of phosphoric acid and potassium chloride;
E, in step d after the thick solution filtering of potassium dihydrogen phosphate, it is 6 that potassium hydroxide is added into filtrate and adjusts pH value of solution, and it is heavy to stand Impurity is filtered off after drop obtains potassium dihydrogen phosphate essence solution;
In f: Xiang Shangshu potassium dihydrogen phosphate essence solution plus purifying phosphoric acid adjusts pH as 4-5, and acquired solution condensing crystallizing, is done filtering Dry to obtain potassium dihydrogen phosphate product, filtrate is potassium dihydrogen phosphate mother liquor.
2. using the method for Wet-process Phosphoric Acid Production potassium dihydrogen phosphate according to claim 1, it is characterised in that: chlorination in step d P in potassium and extract liquor2O5Molar ratio between 1.03-1.05, reaction temperature be 50-70 DEG C, reaction time 20-40min.
3. using the method for Wet-process Phosphoric Acid Production potassium dihydrogen phosphate according to claim 1, it is characterised in that: the extraction in step c P in extraction raffinate2O5Content is 18-20%, is subsequently used for the production of phosphorus ammonium or slurry-spraying pelletizing compound fertilizer.
4. using the method for Wet-process Phosphoric Acid Production potassium dihydrogen phosphate according to claim 1, it is characterised in that: rich into step d It is 7-8 that ammonium hydroxide is added in the organic phase of hydrochloric and a small amount of phosphoric acid and potassium chloride and adjusts pH, and reaction temperature is 50-70 DEG C, reaction Time is 20-40min, stands split-phase, and lower liquid is concentrated to give N P and K ternary compound fertilizer byproduct;Upper layer is extractant phase, It is recycled as the extractant in step c.
5. using the method for Wet-process Phosphoric Acid Production potassium dihydrogen phosphate according to claim 1, it is characterised in that: the phosphorus in step f The reaction of extraction split-phase is carried out in acid dihydride potassium mother liquor return step d.
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CN107758637B (en) * 2017-11-13 2020-12-18 贵阳开磷化肥有限公司 Method for producing industrial-grade potassium dihydrogen phosphate by wet-process phosphoric acid micro-reaction
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

Citations (6)

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CN1789117A (en) * 2004-12-14 2006-06-21 自贡鸿鹤化工股份有限公司 Method for producing potassium dihydrogen phosphate and gypsum using hydrochloric acid method
CN1830762A (en) * 2006-03-30 2006-09-13 云南省化工研究院 Method of continuously preparing potassium dihydrogen phosphate
CN101007626A (en) * 2007-01-25 2007-08-01 黄尚勋 Method for producing phosphate by wet method phosphoric acid purification and hydrochloric acid decomposition for phosphate ore
CN103072963A (en) * 2012-12-28 2013-05-01 山东金正大生态工程股份有限公司 Method for producing potassium dihydrogen phosphate through wet-process phosphoric acid
CN103879981A (en) * 2014-03-19 2014-06-25 钟林 Method for preparing potassium dihydrogen phosphate by using extraction residual acid of phosphoric acid
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

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1789117A (en) * 2004-12-14 2006-06-21 自贡鸿鹤化工股份有限公司 Method for producing potassium dihydrogen phosphate and gypsum using hydrochloric acid method
CN1830762A (en) * 2006-03-30 2006-09-13 云南省化工研究院 Method of continuously preparing potassium dihydrogen phosphate
CN101007626A (en) * 2007-01-25 2007-08-01 黄尚勋 Method for producing phosphate by wet method phosphoric acid purification and hydrochloric acid decomposition for phosphate ore
CN103072963A (en) * 2012-12-28 2013-05-01 山东金正大生态工程股份有限公司 Method for producing potassium dihydrogen phosphate through wet-process phosphoric acid
CN103879981A (en) * 2014-03-19 2014-06-25 钟林 Method for preparing potassium dihydrogen phosphate by using extraction residual acid of phosphoric acid
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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