CN104058378B - The method of monoammonium phosphate and magnesium ammonium phosphate is produced with the acid of wet method concentrated phosphoric acid slag - Google Patents

The method of monoammonium phosphate and magnesium ammonium phosphate is produced with the acid of wet method concentrated phosphoric acid slag Download PDF

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CN104058378B
CN104058378B CN201410325000.9A CN201410325000A CN104058378B CN 104058378 B CN104058378 B CN 104058378B CN 201410325000 A CN201410325000 A CN 201410325000A CN 104058378 B CN104058378 B CN 104058378B
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phosphoric acid
monoammonium phosphate
slag
phosphate
gained
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CN104058378A (en
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马健
李庆
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KUNMING LONGXIANG CHEMICAL CO Ltd
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Abstract

The invention provides the method that monoammonium phosphate and magnesium ammonium phosphate are produced in the acid of a kind of wet method concentrated phosphoric acid slag, with the acid of concentrated phosphoric acid slag for raw material, sized mixing by diluted settlement, defluorinate, the neutralization of segmentation multistep, condensing crystal, mother liquor adjust pH, filter cake and a secondary mother liquid, add in magnesia powder and etc. technique obtain Sodium Silicofluoride, industrial grade monoammonium phosphate and magnesium ammonium phosphate respectively.This technological equipment investment is little, and production cost is low, good product quality, has both solved the problem that the acid of ammonium phosphate enterprises slag can only produce low value-added product, can obtain again industrial grade monoammonium phosphate with low cost and inexpensive slow-release fertilizer magnesium ammonium phosphate.

Description

The method of monoammonium phosphate and magnesium ammonium phosphate is produced with the acid of wet method concentrated phosphoric acid slag
Technical field
The present invention relates to the production method of a kind of monoammonium phosphate and magnesium ammonium phosphate, the method for especially a kind of wet method concentrated phosphoric acid slag acid manufacture level monoammonium phosphate and technical grade and agricultural grade magnesium ammonium phosphate, belongs to chemical technology field.
Background technology
In the production process adopting method of enrichment explained hereafter phosphorus ammonium, the acid of a considerable amount of concentrated phosphoric acid slag will be produced, the dregginess of this phosphoric acid slag acid is higher, the insoluble phosphorus of water is also very high, thus prior art mostly can only produce the low value common fertilizer of the glut the markets such as double superhosphate, double superphosphate or agricultural grade nitre phosphorus ammonium with the acid of phosphoric acid slag, the economic worth not only produced is not high, but also causes a large amount of of this kind of conventional products to overstock.If by prior art by phosphoric acid slag acid direct production phosphorus ammonium, will the quality of product be had a strong impact on.Therefore, be necessary to research and develop the production technique that the acid of concentrated phosphoric acid slag can be utilized to produce high value added product.
Summary of the invention
The acid of a kind of concentrated phosphoric acid slag is the object of the present invention is to provide to produce the method for industrial grade monoammonium phosphate and technical grade and agricultural grade magnesium ammonium phosphate.
The present invention utilizes the low value-added concentrated phosphoric acid slag acid produced in phosphorus ammonium production process to come the industrial grade monoammonium phosphate of production high added value and technical grade and agricultural grade slow-release fertilizer---magnesium ammonium phosphate, be intended to the production potential fully excavating Wet Processes of Phosphoric Acid, the production of full water-soluble phosphate fertilizer and slow-release fertilizer is realized, to meet modern installations agricultural to industrial grade monoammonium phosphate and technical grade and agricultural grade slow-release fertilizer---the demand of magnesium ammonium phosphate with lower cost.
The present invention by by phosphoric acid slag acid dilution, sedimentation, the neutralization of segmentation multistep, condensing crystal, after a mother liquor processing industry level phosphoric acid adjust pH again condensing crystal, each section of filter cake and secondary mother liquid unify to mix size mixing after to add in magnesia powder and etc. technique, obtain industrial grade monoammonium phosphate and technical grade and agricultural grade magnesium ammonium phosphate product.
Core technology of the present invention is; First by after concentrated phosphoric acid slag acid dilution, settlement separate go out clarified acid and sedimentation slag, wherein clarified acid ordinary method neutralizes, sedimentation slag then adopts the phosphorus ammonium mixing solutions of high ph-values as neutralizing agent, thus the neutralization of sedimentation slag is completed with lower neutral temperature and higher liquid-solid ratio, and the mother liquor utilizing manufacture level monoammonium phosphate to produce and a small amount of PHOSPHORIC ACID TECH.GRADE, secondary concentration and crystallization is carried out after carrying out adjusted to ph, and after secondary mother liquid and each section of phosphor ammonium slurry filter cake size mixing, add light-burning magnesium powder, magnesium ammonium phosphate fertilizer can be produced.
Concrete technical scheme of the present invention is: the method for monoammonium phosphate and magnesium ammonium phosphate is produced in a kind of wet method concentrated phosphoric acid slag acid, it is characterized in that comprising following process steps:
A, by the water-soluble P of wet method concentrated phosphoric acid slag acid 2o 5concentration dilution, to 18-22wt%, is settled down to and isolates dilute phosphoric acid liquid and sedimentation slag;
In B, the dilute phosphoric acid liquid that obtains in step A, by Na: the mol ratio of the F=1:3 in dilute phosphoric acid liquid, add sodium carbonate or sodium hydroxide, stirring reaction 60 ~ 100 minutes under normal temperature, filter to obtain phosphoric acid defluorination liquid and filter residue, filter residue is Sodium Silicofluoride product after washing, drying, and washing water are incorporated in phosphoric acid defluorination filtrate;
C, in step B gained part phosphoric acid defluorination liquid, adding liquefied ammonia or bicarbonate of ammonia, to carry out first time neutralization reaction be 4.5 ~ 5.0 to pH value, filters to obtain monoammonium phosphate solution and filter cake;
D, in step C gained monoammonium phosphate solution, continuing to add liquefied ammonia or bicarbonate of ammonia, to carry out second time neutralization reaction to pH value be 5.8 ~ 6.2, filter to obtain de-magging monoammonium phosphate, diammonium phosphate mixing solutions and filter residue, filter residue, after washing, drying, is magnesium ammonium phosphate product;
E, D step gained mixing solutions to be joined in the sedimentation slag of step A gained, and to carry out third time neutralization reaction with liquefied ammonia or ammonium hydrogencarbonate be 4.5 ~ 5.0 to the pH value of sedimentation slag, filter to obtain the monoammonium phosphate solution of purification and filter cake;
F, E step gained purification monoammonium phosphate solution in, continuing to add liquefied ammonia or bicarbonate of ammonia, to carry out the 4th neutralization reaction to pH value be 5.8 ~ 6.2, filter to obtain de-magging monoammonium phosphate, diammonium phosphate mixing solutions and filter residue, filter residue, after washing, drying, is magnesium ammonium phosphate product;
G, to be joined in the remaining phosphoric acid defluorination liquid of step B gained by F step gained mixing solutions, and add appropriate liquefied ammonia or bicarbonate of ammonia, carrying out the 5th neutralization reaction is 4.6 ~ 4.8 to pH value, filters to obtain monoammonium phosphate solution and filter cake;
H, G step gained monoammonium phosphate solution is condensed into P 2o 5mass concentration is the concentrated solution of 28 ~ 32%, is cooled to 60 ~ 75 DEG C, adds appropriate monoammonium phosphate crystal seed routinely, and below crystallisation by cooling to 30 DEG C, filter to isolate crystal and a mother liquor, crystal is industrial grade monoammonium phosphate product after drying;
In I, a mother liquor filtering to isolate in H step, the pH value adding PHOSPHORIC ACID TECH.GRADE to time mother liquor is after 4.6 ~ 4.8, proceed concentrated, the crystallization of H step, filtering separation process, crystal is industrial grade monoammonium phosphate product after drying, and mother liquor is secondary mother liquid;
J, secondary mother liquid I step filtered to isolate, mix with the filter cake of step C, E step, G step gained and size mixing, and add magnesia powder in mixed slurry, after popular response, slaking, drying, obtain agricultural grade magnesium ammonium phosphate.
The wet method concentrated phosphoric acid slag acid of described step A is the P produced in method of enrichment phosphorus ammonium production process 2o 5the slag acid of the wet method concentrated phosphoric acid that mass concentration is 40 ~ 50%, dregginess is 20-30%.
The object of first, second neutralization reaction in described C, D step is the de-magging neutralizer in order to obtain high ph-values, for the third time neutralization reaction of E step creates conditions, avoids the impurity in sedimentation slag to separate out under high temperature neutralization reaction.
4th neutralization reaction of described F step is the magnesium in order to deviate from wherein.
5th neutralization reaction of described G step is in order to the de-magging monoammonium phosphate of the high ph-values by F step and diammonium phosphate solution are adjusted to the monoammonium phosphate solution of low ph value.
The sodium carbonate added in described step B or sodium hydroxide are commercial technical grade product.
The bicarbonate of ammonia added in described step B and step C or liquefied ammonia are commercial technical grade product.
Drying in described step B, D step, F step, H step, I step, J step is conventional drying.
The crystallization of described H step, I step is conventional crystallization.
The magnesia powder added in described J step is that what obtain with magnesite calcining take activated magnesia as the light-magnesite powder of main component.
Without the % of specified otherwise in the present invention, be quality %.
Technological difficulties of the present invention are: how to be separated the water-soluble phosphorus in the acid of wet method concentrated phosphoric acid slag and water-insoluble phosphorus; And how neutralization reaction is carried out to slag acid.
1) viscosity factor due to the acid of wet method concentrated phosphoric acid slag is higher, and solid particulate in the acid of phosphoric acid slag is smaller, therefore cannot come effectively to carry out solid-liquor separation to the acid of phosphoric acid slag with conventional filtration process (as centrifuging, vacuum filtration, filter press etc.).And by after the dilution of step A of the present invention, sedimentation, just can carry out solid-liquor separation to the acid of phosphoric acid slag easily, obtain sedimentation slag and dilute phosphoric acid clear liquor;
2) in addition, to the sedimentation slag of step A, if directly react with liquefied ammonia and sedimentation slag, both react the reaction heat produced, by a large amount of stripping of compound phosphoric acid salt impurity that the fluorine made in sedimentation slag, aluminium, iron, magnesium, manganese etc. and phosphoric acid are formed, then separate out from fat crystal nucleus with the great tertiary iron phosphate of specific surface area and aluminum phosphate etc., and then significantly promote the viscosity of ammonification slip, make it to stir and to filter, finally cannot normally produce.And the present invention why with the de-magging monoammonium phosphate of the high ph-values after first, second neutralization reaction, diammonium phosphate mixing solutions as neutralizing agent, third time neutralization reaction is carried out to the sedimentation slag of step A, the de-magging monoammonium phosphate of high ph-values, diammonium phosphate mixing solutions will be utilized exactly can not to produce the feature of high heat as neutralizing agent, the neutralization reaction fundamentally solved in prior art (directly using liquefied ammonia) is too high because there is reaction heat, thus causes the difficult problem that slip viscosity strengthens, cannot stir, cannot filter; And after the process of sedimentation slag by above-mentioned neutralization reaction, the specific surface area of solid phase particles thing wherein is significantly reduced, thus the strainability of slip is greatly improved.
In a word, adopt the present invention, finally make the neutralization of phosphoric acid slag acid and solid-liquor separation become possibility.Water-soluble phosphorus in slag acid is by the industrial grade monoammonium phosphate Water soluble fertilizer of major part for the production of high added value, water-insoluble phosphorus in slag acid then will fully demonstrate it for the production of slow-release fertilizer and be worth (Water soluble fertilizer and slow-release fertilizer are all market high value added product in short supply at present, and then economic benefit is not good both to be mixed in the common fertilizer of a piece).
The present invention compared with prior art, has following advantages and effect:
1, can not rely on the support of other system, only lean on the system of self just can complete the production process of all products, existing technique needs other system to support the acid of digestion slag;
2, original technology low value-added product that the market such as monoammonium phosphate, coarse whiting, double superphosphate, agricultural grade nitre phosphorus ammonium of phosphoric acid slag acid production agricultural grade can only be utilized superfluous, deficiency in economic performance.The high-quality industrial grade monoammonium phosphate that the present invention then can utilize the acid of phosphoric acid slag to come production market is badly in need of and slow-release fertilizer magnesium ammonium phosphate, added value is high, good in economic efficiency;
3, utilize the high ph-values of de-magging to mix ammonium phosphate solution and carry out Neutralization settlement slag as neutralizing agent, both the problem of reaction heat had been solved, solve again the problem that the too low slip of sedimentation slag liquid-solid ratio is difficult to stir, making to carry out purification slag acid with technique in utilization routine becomes possibility;
4, the present invention adopts the technique of a mother liquor PHOSPHORIC ACID TECH.GRADE adjust pH, significantly simplifies the treatment process of a mother liquor, also significantly improves the rate of recovery of technical grade phosphorus ammonium.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
A, get certain phosphate fertilizer plant wet method concentrated phosphoric acid slag acid 3000 grams (wherein: P 2o 543.04%; F1.99%; SO 36.65%; CaO3.15%; MgO2.12%; Fe 2o 33.30%; AL 2o 32.21%; Containing solid thing 2.20%), add water 3000 grams of agitation and dilutions, stir evenly rear standing sedimentation 24 hours.Siphon must clarify diluted acid 4165 grams, and bottom sedimentation slag stays for subsequent use.
B, in step A gained clarification diluted acid, slowly add 21 grams, technical grade sodium carbonate, under stirring at normal temperature, fully reaction filtered to isolate filtrate and filter residue after 1 hour, with moisture, filter residue was washed till no acidic post-drying and obtained 21 grams of Sodium Silicofluoride product (Na 2siF 6content 95.10%), washing water are incorporated in phosphoric acid defluorination filtrate, obtain defluorinate dilute phosphoric acid 4185 grams;
C, get step B gained defluorinate dilute phosphoric acid 3315 grams, slowly add technical grade bicarbonate of ammonia under stirring at normal temperature and carry out filtering separation after first time neutralization reaction to pH value 4.6, filtrate is monoammonium phosphate solution, and filter cake is for subsequent use;
D, step C gained filtrate is continued to add technical grade bicarbonate of ammonia under stirring at normal temperature carry out second time neutralization reaction to pH value 6.0, continue to stir and fully react filtering separation after 1 hour, namely filter residue obtains fine sand shape magnesium ammonium phosphate product 17 grams (wherein: P after routine washing, drying 2o 533.68%; MgO16.00%; N5.72%), filtrate is monoammonium phosphate, diammonium phosphate mixing solutions after de-magging;
E, the whole filtrate of D step gained slowly joined in step A gained sedimentation slag under stirring at normal temperature and carries out third time neutralization reaction, continuing to add technical grade bicarbonate of ammonia to pH value is 4.6, filtering separation, filter cake is for subsequent use, and filtrate is purifying phosphoric acid one ammonium solution;
F, E step gained purifying phosphoric acid one ammonium solution is continued to add technical grade bicarbonate of ammonia under stirring at normal temperature carry out the 4th neutralization reaction to pH value 6.0, continue to stir and fully react filtering separation after 1 hour, namely filter residue obtains fine sand shape magnesium ammonium phosphate product 71 grams (wherein: P after routine washing, drying 2o 532.97%; MgO16.10%; N5.80%), filtrate is monoammonium phosphate, diammonium phosphate mixing solutions after de-magging;
G, the whole filtrate of F step gained slowly to be joined under stirring at normal temperature in the remaining 870 grams of defluorinate dilute phosphoric acids of step B gained and carry out the 5th neutralization reaction, adding rear pH value is 4.6, filtering separation, and filter cake is for subsequent use, and filtrate is purifying phosphoric acid one ammonium solution;
H, by D step gained purifying phosphoric acid one ammonium solution through conventional evaporation concentration to P 2o 5content is be cooled to 73 DEG C after 31.5%, and add 1 gram of monoammonium phosphate crystal seed, isothermal crystal is decrease temperature crystalline after 1 hour, centrifugation crystal and mother liquor after being cooled to 26 DEG C.Industrial grade monoammonium phosphate product 728 grams is obtained (wherein: P after the drying of gained crystal 2o 561.05%; N12.04%; Water-insoluble 0.01%).Mother liquid obtained is a mother liquor;
I, in H step gained mother liquor, add industrial phosphoric acid to pH value be 4.6, by the process repetitive operation 1 time of evaporation concentration post crystallization, centrifugation in H step, after the drying of gained crystal industrial grade monoammonium phosphate product 290 grams (wherein: P 2o 559.40%; N11.79%; Water-insoluble 0.12%).Mother liquid obtained is secondary mother liquid;
J, to size mixing mother liquid obtained for I step for secondary mother liquid mixes with the filter cake of step C, E step, G step gained, and in mixed slurry, add light-burning magnesium powder 382 grams (containing MgO75.04%), obtain agricultural grade magnesium ammonium phosphate 2120 grams (wherein: P after reaction slaking drying 2o 530.48%; MgO15.79%; N5.68%) embodiment 2
A, get certain phosphate fertilizer plant wet method concentrated phosphoric acid slag acid 3000 grams (wherein: P 2o 543.04%; F1.99%; SO 36.65%; CaO3.15%; MgO2.12%; Fe 2o 33.30%; AL 2o 32.21%; Containing solid thing 2.20%), add water 3000 grams of agitation and dilutions, stir evenly rear standing sedimentation 24 hours.Siphon must clarify diluted acid 4165 grams, and bottom sedimentation slag stays for subsequent use.
B, in step A gained clarification diluted acid, slowly add 16 grams, technical grade sodium hydroxide, under stirring at normal temperature, fully reaction filtered to isolate filtrate and filter residue after 1 hour, with moisture, filter residue was washed till no acidic post-drying and obtained 21 grams of Sodium Silicofluoride product (Na 2siF 6content 95.02%), washing water are incorporated in phosphoric acid defluorination filtrate, obtain defluorinate dilute phosphoric acid 4192 grams;
C, get step B gained defluorinate dilute phosphoric acid 3370 grams, slowly add liquefied ammonia under stirring at normal temperature and carry out filtering separation after first time neutralization reaction to pH value 4.8, filtrate is monoammonium phosphate solution, and filter cake is for subsequent use;
D, step C gained filtrate is under agitation continued to add liquefied ammonia carry out second time neutralization reaction to pH value 6.1, continue to stir fully reaction filtering separation after 1 hour, namely filter residue obtains fine sand shape magnesium ammonium phosphate product 18 grams (wherein: P after routine washing, drying 2o 533.53%; MgO16.04%; N5.74%; ), filtrate is the monoammonium phosphate after de-magging, diammonium phosphate mixing solutions;
E, the whole filtrate of D step gained slowly to be joined under stirring at normal temperature in step A gained sedimentation slag and carry out third time neutralization reaction, continuing to add liquefied ammonia to pH value is 4.8, filtering separation, and filter cake is for subsequent use, and filtrate is purifying phosphoric acid one ammonium solution;
F, E step gained purifying phosphoric acid one ammonium solution is under agitation continued to add liquefied ammonia carry out the 4th neutralization reaction to pH value 6.1, continue to stir and fully react filtering separation after 1 hour, namely filter residue obtains fine sand shape magnesium ammonium phosphate product 73 grams (wherein: P after routine washing, drying 2o 532.91%; MgO16.14%; N5.81%; ), filtrate is the monoammonium phosphate after de-magging, diammonium phosphate mixing solutions;
G, the whole filtrate of F step gained slowly to be joined under stirring at normal temperature in the remaining 822 grams of defluorinate dilute phosphoric acids of step B gained and carry out the 5th neutralization reaction, adding rear pH value is 4.7, filtering separation, and filter cake is for subsequent use, and filtrate is purifying phosphoric acid one ammonium solution;
H, by D step gained purifying phosphoric acid one ammonium solution through conventional evaporation concentration to P 2o 5content is be cooled to 68 DEG C after 31.0%, and add 1 gram of monoammonium phosphate crystal seed, isothermal crystal is decrease temperature crystalline after 1 hour, centrifugation crystal and mother liquor after being cooled to 25 DEG C.Industrial grade monoammonium phosphate product 701 grams is obtained (wherein: P after the drying of gained crystal 2o 561.08%; N12.04%; Water-insoluble 0.01%).Mother liquid obtained is a mother liquor;
I, in H step gained mother liquor, add industrial phosphoric acid to pH value be 4.7, by the process repetitive operation 1 time of evaporation concentration post crystallization, centrifugation in H step, after the drying of gained crystal industrial grade monoammonium phosphate product 289 grams (wherein: P 2o 559.43%; N11.82%; Water-insoluble 0.11%).Mother liquid obtained is secondary mother liquid;
J, to size mixing mother liquid obtained for I step for secondary mother liquid mixes with the filter cake of step C, E step, G step gained, and in mixed slurry, add light-burning magnesium powder 415 grams (containing MgO75.04%), obtain agricultural grade magnesium ammonium phosphate 2210 grams (wherein: P after reaction slaking drying 2o 530.70%; MgO16.13%; N5.17%).

Claims (1)

1. produce a method for monoammonium phosphate and magnesium ammonium phosphate with the acid of wet method concentrated phosphoric acid slag, it is characterized in that comprising following process steps:
A, by the water-soluble P of wet method concentrated phosphoric acid slag acid 2o 5concentration dilution, to 18-22wt%, is settled down to and isolates dilute phosphoric acid liquid and sedimentation slag;
In B, the dilute phosphoric acid liquid that obtains in step A, by Na: the mol ratio of the F=1:3 in dilute phosphoric acid liquid, add sodium carbonate or sodium hydroxide, stirring reaction 60 ~ 100 minutes under normal temperature, filter to obtain phosphoric acid defluorination liquid and filter residue, filter residue is Sodium Silicofluoride product after washing, drying, and washing water are incorporated in phosphoric acid defluorination filtrate;
C, in step B gained part phosphoric acid defluorination liquid, adding liquefied ammonia or bicarbonate of ammonia, to carry out first time neutralization reaction be 4.5 ~ 5.0 to pH value, filters to obtain monoammonium phosphate solution and filter cake;
D, in step C gained monoammonium phosphate solution, continuing to add liquefied ammonia or bicarbonate of ammonia, to carry out second time neutralization reaction to pH value be 5.8 ~ 6.2, filter to obtain de-magging monoammonium phosphate, diammonium phosphate mixing solutions and filter residue, filter residue, after washing, drying, is magnesium ammonium phosphate product;
E, D step gained mixing solutions to be joined in the sedimentation slag of step A gained, and to carry out third time neutralization reaction with liquefied ammonia or ammonium hydrogencarbonate be 4.5 ~ 5.0 to the pH value of sedimentation slag, filter to obtain the monoammonium phosphate solution of purification and filter cake;
F, E step gained purification monoammonium phosphate solution in, continuing to add liquefied ammonia or bicarbonate of ammonia, to carry out the 4th neutralization reaction to pH value be 5.8 ~ 6.2, filter to obtain de-magging monoammonium phosphate, diammonium phosphate mixing solutions and filter residue, filter residue, after washing, drying, is magnesium ammonium phosphate product;
G, to be joined in the remaining phosphoric acid defluorination liquid of step B gained by F step gained mixing solutions, and add appropriate liquefied ammonia or bicarbonate of ammonia, carrying out the 5th neutralization reaction is 4.6 ~ 4.8 to pH value, filters to obtain monoammonium phosphate solution and filter cake;
H, G step gained monoammonium phosphate solution is condensed into P 2o 5mass concentration is the concentrated solution of 28 ~ 32%, is cooled to 60 ~ 75 DEG C, adds appropriate monoammonium phosphate crystal seed routinely, and below crystallisation by cooling to 30 DEG C, filter to isolate crystal and a mother liquor, crystal is industrial grade monoammonium phosphate product after drying;
In I, a mother liquor filtering to isolate in H step, the pH value adding PHOSPHORIC ACID TECH.GRADE to time mother liquor is after 4.6 ~ 4.8, proceed concentrated, the crystallization of H step, filtering separation process, crystal is industrial grade monoammonium phosphate product after drying, and mother liquor is secondary mother liquid;
J, secondary mother liquid I step filtered to isolate, mix with the filter cake of step C, E step, G step gained and size mixing, and add magnesia powder in mixed slurry, after popular response, slaking, drying, obtain agricultural grade magnesium ammonium phosphate.
CN201410325000.9A 2014-07-09 2014-07-09 The method of monoammonium phosphate and magnesium ammonium phosphate is produced with the acid of wet method concentrated phosphoric acid slag Active CN104058378B (en)

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CN105731407B (en) * 2016-04-11 2018-04-27 河南师范大学 The method of Wet-process Phosphoric Acid Production ammonium dihydrogen phosphate
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