CN110371944A - A kind of method of purifying phosphoric acid raffinate and six hypophosphite monohydrate ammonium magnesium of recycling - Google Patents
A kind of method of purifying phosphoric acid raffinate and six hypophosphite monohydrate ammonium magnesium of recycling Download PDFInfo
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- CN110371944A CN110371944A CN201910684701.4A CN201910684701A CN110371944A CN 110371944 A CN110371944 A CN 110371944A CN 201910684701 A CN201910684701 A CN 201910684701A CN 110371944 A CN110371944 A CN 110371944A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
- C01B25/451—Phosphates containing plural metal, or metal and ammonium containing metal and ammonium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01P2006/80—Compositional purity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The present invention relates to a kind of methods of six hypophosphite monohydrate ammonium magnesium of purifying phosphoric acid raffinate and recycling.Its technical solution is: by phosphoric acid raffinate: the mass ratio of water is 1: the water is added in the phosphoric acid raffinate, stirs 0.5~1h, the phosphoric acid raffinate after being diluted under normal temperature conditions by (0.1~0.3);Press urea again: the mass ratio of the phosphoric acid raffinate after the dilution is that (urea is added in the phosphoric acid raffinate after the dilution 0.5~2) ︰ 1, and stirring to pH value is 5~6 under the conditions of 70~100 DEG C, it is cooling, it is separated by solid-liquid separation, washing, obtains except iron molten aluminum and containing iron aluminum slag;Then described will remove iron molten aluminum and be stirred under the conditions of 70~100 DEG C to pH value is 6~7, cooling, is separated by solid-liquid separation, washing obtains phosphoric acid raffinate scavenging solution and six hypophosphite monohydrate ammonium magnesium.It is easy to be recycled that the present invention has the characteristics that process flow is short, phosphorus loses small and metal ion.
Description
Technical field
The invention belongs to phosphoric acid raffinate technical fields.More particularly to six hydration phosphorus of a kind of purifying phosphoric acid raffinate and recycling
The method of sour ammonium magnesium.
Background technique
Phosphoric acid is the important intermediate products of sulphur dioxide of phosphor chemical industry, is widely used in fertilizer, food, medicine and other chemical industry neck
Domain.The production of phosphoric acid is broadly divided into thermal method and wet process.The energy consumption that thermal method produces phosphoric acid is higher, is mainly used to produce high-purity, height
Value-added product;And though Wet-process phosphoric acid (WPPA) energy consumption is lower, in production process a large amount of impurity such as Fe, Al, Mg plasmas with
Phosphorus enters leachate, causes subsequent phosphorus to separate with foreign ion more difficult.Although phosphoric acid by wet process solvent extraction technology has aobvious
The economic benefit of work, but there are following two main problems: and first is that extraction process phosphorus is extracted, foreign ion is enriched with, raffinate
Sour viscosity is very big, a large amount of gelatinous precipitates occurs, directly filter it is extremely difficult, industry in frequently with plate and frame filter press filter,
But efficiency is lower;Second is that still containing certain density phosphorus in raffinate, it is commonly used to produce agricultural monoammonium phosphate or Diammonium phosphate (DAP),
But the impurity ion contents such as Fe, Al, Mg are very high, cause subsequent phosphorus product purity not up to standard, to the recycling of phosphorus in raffinate
Bring certain difficulty.
" the raffinate method that neutralisation prepares industrial grade monoammonium phosphate twice " (CN103896232 A) patented technology and old
Abiding by road etc., (the raffinate such as Chen Zunkui prepares the work of industrial grade monoammonium phosphate using ammonia neutralisation processing twice phosphoric acid raffinate
Skill optimizes [J], chemistry and bioengineering, 2015,32 (08), 63~66), PHOSPHORIC ACID TECH.GRADE one is finally prepared using crystallisation
Ammonium: high viscosity raffinate is diluted first;Then the raffinate first time ammonia after dilution is neutralized, is neutralized for the first time
Terminal pH is 3.4~3.6, is filtered after curing;Second of ammonia neutralization is carried out again, the second terminal pH that neutralizes is 4.4~
4.6, it is filtered after curing;Monoammonium phosphate is finally prepared using concentrated crystallization.The technique is using conventional nertralizer-ammonia processing extraction
Remaining phosphoric acid, though impurity-eliminating effect is preferably, there are still following three problems: first is that a large amount of gelatinous precipitates are generated in dedoping step,
Phosphorus loss is big, commonly reaches 25~30%;Second is that neutralization precipitation slag purity is not high twice, it is difficult to the magnesium in raffinate phosphoric acid from
Son is comprehensively utilized;Third is that being cleaned using ammonia, operating process is difficult to avoid that ammonia is escaped from reactor, laboratory and work
Industry execute-in-place environment is poor.
" a method of using melamine purifying phosphoric acid raffinate disodium hydrogen phosphate " (105584998 A of CN) is special
Sharp technology, the technology, as precipitating reagent, clean to phosphoric acid by wet process raffinate, generate in dedoping step using melamine
The double salt of melamine, and recycled with double salt of the sodium carbonate to melamine, though finally obtained disodium hydrogen phosphate, the work
The melamine that skill is added is expensive and consumption is big, and cannot recycle to the magnesium ion in solution.
" technique of removing magnesium from phosphoric acid residue " (102583302 A of CN) patented technology and the superfine solvent that is respectively adopted of Lian Pei extract
It follows the example of with the magnesium ion in ion-exchange removal phosphoric acid raffinate (in the superfine Wet-Process Phosphoric Acid Solution by Ion Exchange Technique of Lian Pei
Magnesium ion [J], Guizhou University of Technology's journal, 2008,37 (1), 36~39), obtain good effect.But it is existing
Solvent extraction can only be handled a certain ion in phosphoric acid raffinate with ion-exchange process, segment processing different impurities
Though feasible in technique, process flow is long, and the phosphorous intermediate product generated is more, reduces the overall recovery of phosphorus.
In conclusion existing phosphoric acid raffinate purification techniques is primarily present, process flow is long, phosphorus loss is big, metal ion
It is difficult to the disadvantages of recycling.
Summary of the invention
The present invention is directed to overcome prior art defect, it is therefore an objective to provide a kind of process flow is short, phosphorus lose small and metal from
The method for the six hypophosphite monohydrate ammonium magnesium of purifying phosphoric acid raffinate and recycling that son easily recycles.
To achieve the above object, the technical solution adopted by the present invention comprises the concrete steps that:
Step 1: dilution
By phosphoric acid raffinate: the mass ratio of water is 1: (0.1~0.3) water is added in the phosphoric acid raffinate,
0.5~1h, the phosphoric acid raffinate after being diluted are stirred under normal temperature condition.
Step 2: removal iron, aluminium
By urea: the mass ratio of the phosphoric acid raffinate after the dilution is that (0.5~2) ︰ 1, will be described in urea addition
In phosphoric acid raffinate after dilution, stirring to pH value is 5~6 under the conditions of 70~100 DEG C, is cooled to room temperature, and is separated by solid-liquid separation, washes
It washs, obtains except iron molten aluminum and containing iron aluminum slag.
Step 3: recycling magnesium
Described will remove iron molten aluminum and be stirred under the conditions of 70~100 DEG C to pH value is 6~7, is cooled to room temperature, is separated by solid-liquid separation,
Washing, obtains phosphoric acid raffinate scavenging solution and six hypophosphite monohydrate ammonium magnesium.
The phosphoric acid raffinate: P2O5Content > 35wt%, content of MgO are 2~8wt%, Al2O3Content is 4~8wt%,
Fe2O3Content is 0.5~3wt%, CaO content < 0.05wt%, K2O content < 0.1wt%, Na2O content < 1.5wt%, solid content
For 4~8wt%, pH value is less than -0.8;The density of phosphoric acid raffinate clear liquid is greater than 1.6g/cm3。
Due to the adoption of the above technical scheme, the present invention has following good effect compared with prior art:
(1) urea is added at one time by the present invention, in two stages decomposing urea, and the first stage is removal iron, aluminium impurity,
Iron, aluminium impurity removal rate up to 98% or more;Second stage is recycling magnesium ion, and magnesium is deposited in the form of seven hypophosphite monohydrate ammonium magnesium
It is in second stage sediment, the purity of seven hypophosphite monohydrate ammonium magnesium reaches 98% or more, and the magnesium rate of recovery reaches 90% or more, can
Directly comprehensive utilization or further purification preparation higher purity product.
(2) urea that the present invention uses can effectively prevent co-precipitation, targetedly go dephosphorization as slow release precipitator
Iron, aluminium impurity in sour raffinate, and recycle magnesium ion, it is therefore prevented that phosphorus is mingled with, and the sediment generated is in powdery, is avoided
The loss late of the generation of conventional ammonium hydroxide purification process gelatinous precipitate, phosphorus can be reduced to 5% or less.The present invention is removed using urea
Foreign ion and the mechanism for inhibiting phosphorus to lose are as follows:
Urea will be slow release ammonia being heated to 60 DEG C or more, and reaction equation is as follows:
CO(NH2)2+H2O→CO2↑+2NH3
NH3+H2O→NH4 ++OH-
The obtained product NH of urea hydrothermal decomposition4 +It is the subsequent reactant for preparing ammonium phosphate salt product, and this reaction life
At OH-The promotion for then facilitating pH value of solution is finally reached the optimum PH range of contamination precipitation in phosphoric acid raffinate.In addition, control
Condition processed decomposes urea slowly, uniformly discharges OH in the solution-, can prevent conventional ammonium hydroxide from adjusting local ph mistake in pH method
Winding that is high and leading to phosphorus caused by the intense hydrolysis of the part Fe, Al.
By surface topography containing iron aluminum slag of the invention and in the prior art ammonium hydroxide removal of impurities slag surface topography compare: this hair
The ammonium hydroxide removal of impurities product of bright urea removal of impurities product compared to the prior art, pattern is more complete uniform, and crystalline size is bigger.?
Useful element phosphorus and magnesium are not easy to be not only reduced the loss of phosphorus by winding in Fe, Al precipitation process, and are the recycling of magnesium
It creates condition.
(3) process object of the invention is muddy phosphoric acid raffinate, directly cleans, is not required to muddy phosphoric acid raffinate
Gelatinous precipitate in filtering phosphoric acid raffinate can realize the purification to phosphoric acid raffinate, the precipitating generated on a microscopic level
Object crystallinity is high, and crystallite dimension is big, and particle is in fine-powdered on a macroscopic level, and the removal of impurities that the removal of impurities mode of the prior art obtains
Jelly, and the muddy object in phosphoric acid raffinate reacts in dedoping step with precipitating reagent slag, so that filter process is easier to carry out,
Shorten process flow.
Therefore, it is easy to be recycled to have the characteristics that process flow is short, phosphorus loses small and magnesium ion by the present invention.
Detailed description of the invention
Fig. 1 is a kind of surface topography SEM figure containing iron aluminum slag of the invention;
Fig. 2 is the surface topography SEM figure of the ammonium hydroxide removal of impurities product of the prior art.
Specific embodiment
The present invention will be further described With reference to embodiment, not to the limitation of its protection scope.
In present embodiment:
The phosphoric acid raffinate: P2O5Content > 35wt%, content of MgO are 2~8wt%, Al2O3Content is 4~8wt%,
Fe2O3Content is 0.5~3wt%, CaO content < 0.05wt%, K2O content < 0.1wt%, Na2O content < 1.5wt%, solid content
For 4~8wt%, pH value is less than -0.8;The density of phosphoric acid raffinate clear liquid is greater than 1.6g/cm3。
It is repeated no more in embodiment.
Embodiment 1
A kind of method of purifying phosphoric acid raffinate and six hypophosphite monohydrate ammonium magnesium of recycling.The specific step of the present embodiment the method
Suddenly it is:
Step 1: dilution
By phosphoric acid raffinate: the mass ratio of water is 1: (0.1~0.15) water is added in the phosphoric acid raffinate,
0.5~0.7h, the phosphoric acid raffinate after being diluted are stirred under normal temperature conditions.
Step 2: removal iron, aluminium
By urea: the mass ratio of the phosphoric acid raffinate after the dilution is that (0.5~1) ︰ 1, will be described in urea addition
In phosphoric acid raffinate after dilution, stirring to pH value is 5~5.4 under the conditions of 70~80 DEG C, is cooled to room temperature, and is separated by solid-liquid separation,
Washing is obtained except iron molten aluminum and containing iron aluminum slag.
Step 3: recycling magnesium
Described will remove iron molten aluminum and be stirred under the conditions of 70~80 DEG C to pH value is 6~6.4, is cooled to room temperature, is separated by solid-liquid separation,
Washing, obtains phosphoric acid raffinate scavenging solution and six hypophosphite monohydrate ammonium magnesium.
Embodiment 2
A kind of method of purifying phosphoric acid raffinate and six hypophosphite monohydrate ammonium magnesium of recycling.The specific step of the present embodiment the method
Suddenly it is:
Step 1: dilution
By phosphoric acid raffinate: the mass ratio of water is 1: (0.15~0.2) water is added in the phosphoric acid raffinate,
0.6~0.8h, the phosphoric acid raffinate after being diluted are stirred under normal temperature conditions.
Step 2: removal iron, aluminium
By urea: the mass ratio of the phosphoric acid raffinate after the dilution is that (1~1.5) ︰ 1, will be described in urea addition
In phosphoric acid raffinate after dilution, stirring to pH value is 5.2~5.6 under the conditions of 80~90 DEG C, is cooled to room temperature, solid-liquid point
From washing is obtained except iron molten aluminum and containing iron aluminum slag.
Step 3: recycling magnesium
Described will remove iron molten aluminum and be stirred under the conditions of 80~90 DEG C to pH value is 6.2~6.6, is cooled to room temperature, solid-liquid point
From washing obtains phosphoric acid raffinate scavenging solution and six hypophosphite monohydrate ammonium magnesium.
Embodiment 3
A kind of method of purifying phosphoric acid raffinate and six hypophosphite monohydrate ammonium magnesium of recycling.The specific step of the present embodiment the method
Suddenly it is:
Step 1: dilution
By phosphoric acid raffinate: the mass ratio of water is 1: (0.2~0.3) water is added in the phosphoric acid raffinate,
0.8~1h, the phosphoric acid raffinate after being diluted are stirred under normal temperature condition.
Step 2: removal iron, aluminium
By urea: the mass ratio of the phosphoric acid raffinate after the dilution is that (1.5~2) ︰ 1, will be described in urea addition
In phosphoric acid raffinate after dilution, stirring to pH value is 5.6~6 under the conditions of 90~100 DEG C, is cooled to room temperature, and is separated by solid-liquid separation,
Washing is obtained except iron molten aluminum and containing iron aluminum slag.
Step 3: recycling magnesium
Described will remove iron molten aluminum and be stirred under the conditions of 90~100 DEG C to pH value is 6.6~7, is cooled to room temperature, solid-liquid point
From washing obtains phosphoric acid raffinate scavenging solution and six hypophosphite monohydrate ammonium magnesium.
Present embodiment has following good effect compared with prior art:
(1) urea is added at one time by present embodiment, in two stages decomposing urea, the first stage be removal iron,
Aluminium impurity, iron, aluminium impurity removal rate up to 98% or more;Second stage is recycling magnesium ion, and magnesium is with seven hypophosphite monohydrate ammonium magnesium
Form be present in second stage sediment, the purity of seven hypophosphite monohydrate ammonium magnesium reaches 98% or more, and the magnesium rate of recovery reaches
90% or more, it can directly comprehensively utilize or further purify preparation higher purity product.
(2) urea that present embodiment uses can effectively prevent co-precipitation, specific aim as slow release precipitator
Removal phosphoric acid raffinate in iron, aluminium impurity, and recycle magnesium ion, it is therefore prevented that phosphorus is mingled with, and the sediment generated is in powder
Shape, avoids the generation of conventional ammonium hydroxide purification process gelatinous precipitate, and the loss late of phosphorus can be reduced to 5% or less.This is specific real
Mode is applied using urea precipitation foreign ion and inhibits the mechanism of phosphorus loss are as follows:
Urea will be slow release ammonia being heated to 60 DEG C or more, and reaction equation is as follows:
CO(NH2)2+H2O→CO2↑+2NH3
NH3+H2O→NH4 ++OH-
The obtained product NH of urea hydrothermal decomposition4 +It is the subsequent reactant for preparing ammonium phosphate salt product, and this reaction life
At OH-The promotion for then facilitating pH value of solution is finally reached the optimum PH range of contamination precipitation in phosphoric acid raffinate.In addition, control
Condition processed decomposes urea slowly, uniformly discharges OH in the solution-, can prevent conventional ammonium hydroxide from adjusting local ph mistake in pH method
Winding that is high and leading to phosphorus caused by the intense hydrolysis of the part Fe, Al.
By the surface topography containing iron aluminum slag of present embodiment and ammonium hydroxide removal of impurities slag surface topography progress in the prior art
Comparison, as a result as depicted in figs. 1 and 2: Fig. 1 is a kind of surface topography SEM figure containing iron aluminum slag of embodiment 1;Fig. 2 is existing skill
The surface topography SEM figure of ammonium hydroxide removal of impurities product in art.As shown in Figure 1, the removal of impurities product of present embodiment is flake
It stacks, structural integrity is consistent, it was demonstrated that urea precipitation product crystallinity is high.As shown in Figure 2, the ammonium hydroxide removal of impurities product of the prior art
Sheet granularity is smaller, in irregular shape, easily forms bulky grain and reunites.By the comparison of Fig. 1 and Fig. 2 it is found that present embodiment
Urea removal of impurities product ammonium hydroxide compared to the prior art clean product, pattern is more complete uniform, and crystalline size is bigger.?
Useful element phosphorus and magnesium are not easy to be not only reduced the loss of phosphorus by winding in Fe, Al precipitation process, and are the recycling of magnesium
It creates condition.
(3) process object of present embodiment is muddy phosphoric acid raffinate, direct to muddy phosphoric acid raffinate
Removal of impurities, the gelatinous precipitate being not required in filtering phosphoric acid raffinate can realize the purification to phosphoric acid raffinate, on a microscopic level
The sediment crystallinity of generation is high, and crystallite dimension is big, and particle is in fine-powdered on a macroscopic level, and the removal of impurities mode of the prior art
Jelly, and the muddy object in phosphoric acid raffinate reacts in dedoping step with precipitating reagent obtained removal of impurities slag, so that filtered
Cheng Gengyi is carried out, and shortens process flow.
Therefore, it is easy to be recycled to have the characteristics that process flow is short, phosphorus loses small and magnesium ion for present embodiment.
Claims (2)
1. a kind of method of six hypophosphite monohydrate ammonium magnesium of purifying phosphoric acid raffinate and recycling, it is characterised in that the specific step of the method
Suddenly it is:
Step 1: dilution
By phosphoric acid raffinate: the mass ratio of water is 1: (0.1~0.3) water is added in the phosphoric acid raffinate, in room temperature
Under the conditions of stir 0.5~1h, the phosphoric acid raffinate after being diluted;
Step 2: removal iron, aluminium
By urea: the mass ratio of the phosphoric acid raffinate after the dilution is that (dilution is added in the urea by 0.5~2) ︰ 1
In phosphoric acid raffinate afterwards, stirring to pH value is 5~6 under the conditions of 70~100 DEG C, is cooled to room temperature, and is separated by solid-liquid separation, washing,
It obtains except iron molten aluminum and containing iron aluminum slag;
Step 3: recycling magnesium
Described will remove iron molten aluminum and be stirred under the conditions of 70~100 DEG C to pH value is 6~7, is cooled to room temperature, is separated by solid-liquid separation, washing,
Obtain phosphoric acid raffinate scavenging solution and six hypophosphite monohydrate ammonium magnesium.
2. the method for six hypophosphite monohydrate ammonium magnesium of purifying phosphoric acid raffinate according to claim 1 and recycling, it is characterised in that
The phosphoric acid raffinate: P2O5Content > 35wt%, content of MgO are 2~8wt%, Al2O3Content is 4~8wt%, Fe2O3Content
For 0.5~3wt%, CaO content < 0.05wt%, K2O content < 0.1wt%, Na2O content < 1.5wt%, solid content be 4~
8wt%, pH value are less than -0.8;The density of phosphoric acid raffinate clear liquid is greater than 1.6g/cm3。
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CN101891504A (en) * | 2010-07-26 | 2010-11-24 | 瓮福(集团)有限责任公司 | Method for producing granular monoammonium phosphate with raffinate |
CN102815685A (en) * | 2012-08-10 | 2012-12-12 | 清华大学 | Wet-method phosphoric acid staged extraction and purification process |
CN104058378A (en) * | 2014-07-09 | 2014-09-24 | 昆明隆祥化工有限公司 | Method for producing monoammonium phosphate and magnesium ammonium phosphate by using wet concentrated phosphoric acid residues |
CN105600763A (en) * | 2016-01-22 | 2016-05-25 | 金正大诺泰尔化学有限公司 | Method for producing industrial monoammonium phosphate through fluoride salt purification method |
CA2977986A1 (en) * | 2017-08-30 | 2019-02-28 | Boost Environmental systems Inc. | Process for removal or recovery of ammonium nitrogen from wastewater streams |
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CN1654317A (en) * | 2004-12-24 | 2005-08-17 | 贵州宏福实业开发有限总公司 | Purified wet-process technique for producing phosphoric acid and equipment thereof |
CN101891504A (en) * | 2010-07-26 | 2010-11-24 | 瓮福(集团)有限责任公司 | Method for producing granular monoammonium phosphate with raffinate |
CN102815685A (en) * | 2012-08-10 | 2012-12-12 | 清华大学 | Wet-method phosphoric acid staged extraction and purification process |
CN104058378A (en) * | 2014-07-09 | 2014-09-24 | 昆明隆祥化工有限公司 | Method for producing monoammonium phosphate and magnesium ammonium phosphate by using wet concentrated phosphoric acid residues |
CN105600763A (en) * | 2016-01-22 | 2016-05-25 | 金正大诺泰尔化学有限公司 | Method for producing industrial monoammonium phosphate through fluoride salt purification method |
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