CN109019545A - A kind of technique of phosphoric acid,diluted demetalization ion - Google Patents
A kind of technique of phosphoric acid,diluted demetalization ion Download PDFInfo
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- CN109019545A CN109019545A CN201811058373.9A CN201811058373A CN109019545A CN 109019545 A CN109019545 A CN 109019545A CN 201811058373 A CN201811058373 A CN 201811058373A CN 109019545 A CN109019545 A CN 109019545A
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- phosphoric acid
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- filtrate
- ammonium
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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
- C01B25/18—Phosphoric acid
- C01B25/234—Purification; Stabilisation; Concentration
- C01B25/237—Selective elimination of impurities
- C01B25/238—Cationic impurities, e.g. arsenic compounds
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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
- C01B25/28—Ammonium phosphates
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G1/00—Mixtures of fertilisers belonging individually to different subclasses of C05
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Fertilizers (AREA)
Abstract
The present invention provides a kind of technique of phosphoric acid,diluted demetalization ion, phosphoric acid,diluted is pumped into ammoniation reactor from phosphoric acid,diluted defecator bottom, liquefied ammonia is passed through simultaneously to be reacted, the phosphor ammonium slurry obtained after the reaction was completed is sent into phosphor ammonium slurry storage tank, phosphor ammonium slurry is after filter press filters pressing, phosphorus ammonium filtrate enters hold-up vessel, and is pumped to the storage of phosphoric acid,diluted ageing tank；Phosphorus ammonium filtrate after ageing is sent to enrichment facility after mixing with phosphoric acid,diluted to be concentrated, and gelled acid send to monoammonium phosphate device and produces high-quality Diammonium phosphate (DAP)；Filter residue after ageing send to multi-function device and produces compound fertilizer.Phosphoric acid,diluted ammoniation process reduction impurity content mixes concentration with phosphoric acid,diluted and produces in high-quality Diammonium phosphate (DAP) in the present invention: obtaining clear liquid after diluted acid ammonification filtrate and clarification phosphoric acid,diluted mixing, do not crystallize, mixed liquor is easier to be concentrated in vacuo, after concentrate is cooled to room temperature, sludge precipitating in deacidification is outer, there are also a small amount of ammonium salt crystallizations to be precipitated, therefore solid content is higher.
Description
Technical field
Technical solution of the present invention provides the treatment process of a metal ion species, and metal ion is de- specially in phosphoric acid,diluted
Except technique.
Background technique
As the continuous exploitation of phosphate rock resource utilizes, the impurity such as Fe, Al, Mg in phosphorus ore are gradually risen, and phosphorus ore quality is not
Disconnected decline.During extraction produces phosphoric acid, the metal ions such as Fe, Al, Mg in phosphorus ore are largely dissolved in phosphoric acid phosphorus ore,
Lead to (the R in phosphoric acid2O3+MgO)/P2O5Index (i.e. MER value) increases, the gold such as Fe, Al, Mg when producing Diammonium phosphate (DAP)
Belong to cation and replaces NH4 +Ion reduces nitrogen content, while the metal cations such as Fe, Al, Mg and PO4 3-It is complexed in conjunction with indissoluble is generated
Object reduces water-soluble phosphorus, so as to cause the decline of Diammonium phosphate (DAP) quality.
To guarantee Diammonium phosphate (DAP) quality, high-quality Diammonium phosphate (DAP) is produced, technical solution of the present invention uses phosphoric acid,diluted ammoniation process
Part metals cation in phosphoric acid is removed, the metal cations impurity content such as Fe, Al, Mg in phosphoric acid is reduced, improves phosphoric acid quality.
Summary of the invention
Technical solution of the present invention is reduced in phosphoric acid using part metals cation in phosphoric acid,diluted ammoniation process removing phosphoric acid
The metal cations impurity content such as Fe, Al, Mg improves phosphoric acid quality, produces high-quality Diammonium phosphate (DAP), filter residue is for producing compound
(conjunction) fertilizer or organic and inorganic fertilizer realize the comprehensive utilization of slag acid.
Often containing metal cations impurity such as iron, aluminium, magnesium in phosphoric acid by wet process.In ammonifying process, with degree of neutralization
Improve, be generally neutralized to pH value greater than 2.0, will there are a large amount of sediments to be precipitated, these sediments be mainly iron content, aluminium, magnesium,
The complex precipitate of ammonium, fluorine, phosphorus etc., when such as pH ≈ 4.35, sediment is (Fe, Al) NH4(HPO4)2·0.5H2O、(Fe,Al)
Mg(NH4)2(HPO4)2F3、MgHPO4、CaHPO4Deng.
Phosphoric acid,diluted ammonifying process releases a large amount of heat, can evaporate a part of water removed in phosphor ammonium slurry using it.In
And 1kgNH31~2kgH can be evaporated2O, evaporite ratio are related with phosphoric acid concentration and temperature.
The clarified filtering and removing slag of phosphoric acid,diluted ammonification slurry, removing part metals cation, obtain the preferable phosphoric acid one of quality
Ammonium filtrate.
Monoammonium phosphate filtrate is concentrated with phosphoric acid,diluted as after mixing again, and gelled acid can be used for producing high-quality Diammonium phosphate (DAP),
Improve Diammonium phosphate (DAP) quality.
Filter residue can be used for producing monoammonium phosphate, ammonium phosphate fertiliser containing magnesium, nitro phosphate fertilizer, crop formula fertilizer special, universal NPK etc.
A variety of compound (compound) fertilizer.
Specifically comprises the processes of: using monoammonium phosphate device preneutralization slot as phosphoric acid,diluted ammoniation reactor, come from phosphoric acid,diluted defecator
The phosphoric acid,diluted of underflow is pumped into ammoniation reactor through underground tank, while being passed through liquefied ammonia, carries out aminating reaction, adjusts liquefied ammonia additional amount
Control pH value.Phosphor ammonium slurry sufficiently after reaction is sent into phosphor ammonium slurry storage tank, and phosphor ammonium slurry is after full automatic pressure filter filters pressing, phosphorus
Ammonium filtrate enters hold-up vessel, and is pumped to former phosphoric acid,diluted ageing tank storage.Filter residue send to multi-function device and produces compound fertilizer.
Phosphorus ammonium filtrate is sent to phosphoric acid concentrating device after mixing on delivery pump outlet conduit after metering with phosphoric acid,diluted and is carried out
Concentration, gelled acid send to monoammonium phosphate device and produce high-quality Diammonium phosphate (DAP).
This programme makes full use of existing equipment, mainly optimizes transformation to original tube pass, guarantees that filter press both may be used
It, also can filters pressing phosphoric acid slag with filters pressing phosphor ammonium slurry.
In technical solution of the present invention, the key of phosphoric acid,diluted ammonification removing metal cation is that ammonification slurry process controls
And solid-liquor separation is with phosphoric acid,diluted in order to obtain the more excellent process conditions of phosphoric acid,diluted ammonification, filtering and removing metal cation impurity
Raw material carries out experimental verification evaluation to phosphorus ammonium filtrate and phosphoric acid,diluted mixed acid concentration situation, gelled acid production DAP product quality.
Phosphoric acid,diluted ammonification main technique Con trolling index is as follows:
Phosphoric acid,diluted ammonification slurry: pH=4.0~4.5, time 30min-50min；
Phosphor ammonium slurry digestion time 30-50min, 80 DEG C of filtration temperature；
Phosphorus ammonium filtrate: pH=4.0~4.5；
Phosphorus ammonium filtrate and phosphoric acid,diluted mixed proportion: phosphorus ammonium filtrate accounts for 25~30%, mixed phosphoric acid MER≤0.085；
Ammonification phosphoric acid,diluted concentration: 20%~25%P2O5(22%~23%P2O5Preferably), SO3Content is as low as possible and stablizes
Control；
Mixed acid endpoint concentration: 40-46%P is concentrated2O5, according to DAP production level homeostasis, clarification cannot be aged and (preferably protected
Holding temperature directly send DAP to produce).
Clear liquid is obtained after phosphoric acid,diluted ammonification filtrate and clarification phosphoric acid,diluted mixing, is not crystallized, mixed liquor is easier very
Sky concentration, after concentrate is cooled to room temperature, the sludge precipitating in deacidification is outer, and there are also a small amount of ammonium salt crystallizations to be precipitated, and shows as containing
Gu measuring higher.Therefore concentrate had better not cool down, is aged, clarify when industrial production, directly DAP be sent to produce.In concentration process,
Phosphorus does not lose substantially, nitrogen loss very little, and boiling point is lower than the concentration of pure phosphoric acid.
Phosphoric acid,diluted ammonification filtrate and clarification phosphoric acid,diluted lead in ammonia after being mixed in vacuum and high-quality DAP product can be made.
Ammonification wet cake is proposed to be used in multi-function device composite heat transfer, and additive amount is true by complex fertilizer product specification requirement
It is fixed.
The results showed that using phosphoric acid,diluted ammonification filter reduce impurity content, and with clarification phosphoric acid,diluted mix after again into
Row concentration, gelled acid, which leads to ammonia neutralization, can produce high-quality Diammonium phosphate (DAP).Filter residue can be used for producing compound (compound) fertilizer.
Specific embodiment
Embodiment 1
Phosphoric acid,diluted: the P of phosphoric acid,diluted device production2O5The phosphoric acid,diluted of content 20-25%.
Liquefied ammonia: being supplied by synthesis ammonia plant, and quality will reach GB536-88 standard.
Phosphoric acid,diluted ammonification, filter device ability: 20,000 tons of (100%P2O5)/year.It specifically need to be according to slag ammonification slurry filters pressing feelings
The operation of situations such as condition, DAP washing tail gas pressure determines.
Using monoammonium phosphate device preneutralization slot as phosphoric acid,diluted ammoniation reactor, the phosphoric acid,diluted from phosphoric acid,diluted defecator underflow
It is pumped into ammoniation reactor through underground tank, while being passed through liquefied ammonia, carries out aminating reaction, adjusts liquefied ammonia additional amount, control was reacted
Phosphoric acid,diluted ammonification slurry pH value is 4.0~4.5 in journey, time 30min.Phosphor ammonium slurry sufficiently after reaction is sent into phosphor ammonium slurry
Storage tank, for phosphor ammonium slurry after full automatic pressure filter filters pressing, phosphorus ammonium filtrate enters hold-up vessel, and is pumped to former phosphoric acid,diluted ageing tank
Storage, phosphor ammonium slurry digestion time are 30min, 80 DEG C of filtration temperature, obtain phosphorus ammonium filtrate pH=4.2.Filter residue is sent to multi-functional
Device produces compound fertilizer.
Phosphorus ammonium filtrate is sent to phosphoric acid concentrating device after mixing on delivery pump outlet conduit after metering with phosphoric acid,diluted and is carried out
Concentration, gelled acid send to monoammonium phosphate device and produce high-quality Diammonium phosphate (DAP), control phosphorus ammonium filtrate in mixed liquor and account for 28%, mixed phosphorus
Sour MER is 0.08；Concentration increasing mixed acid concentration is 45%P2O5。
This programme makes full use of existing equipment, mainly optimizes transformation to original tube pass, guarantees that filter press both may be used
It, also can filters pressing phosphoric acid slag with filters pressing phosphor ammonium slurry.
In equipment installation setting in technical solution of the present invention, until preneutralization slot phosphoric acid,diluted feed-line: phosphoric acid,diluted
Lower slot pump discharge pipeline appropriate location increases a threeway and two valves, with a DN100 pipeline and the dense phosphorus of former preneutralization slot
Acid tube line connect (link position is before flowmeter), with underground tank pump by phosphoric acid,diluted defecator underflow phosphoric acid send to preneutralization slot into
Row ammonification.
To phosphor ammonium slurry storage tank phosphor ammonium slurry feed-line: increasing a DN100 shurry pump (variable frequency pump) and be exported to filters pressing
The pipeline of device slurry storage tank installs the flowmeter (being left unused flowmeter with shurry pump to pelletizer) of a DN100.And it is pumping
Outlet configuration DN50 steam blowing pipeline.
To phosphoric acid,diluted ageing tank phosphorus ammonium filtrate feed-line: close to phosphoric acid,diluted ageing tank on former filter press filtrate feed-line
Appropriate position (specific location scene determines) increases a threeway, with a DN80 pipeline to phosphoric acid,diluted ageing tank, installation two
Phosphorus ammonium filtrate is delivered to the storage of phosphoric acid,diluted ageing tank by automatic cutout valve, and when opening dense slag filters pressing, it is clear that filtrate enters concentrated phosphoric acid
Clear slot.The phosphoric acid,diluted for carrying out inherent filtration is directly entered the storage of phosphoric acid,diluted defecator by switch valve.And DN50 is configured in pump discharge
Steam blowing pipeline.
To phosphoric acid concentrating device phosphorus ammonium filtrate feed-line: the phosphoric acid,diluted delivery pump to phosphoric acid concentrating device has two, matches
The outlet line of wherein one suction line and phosphoric acid,diluted ageing tank is attached, and is exporting by a piece DN200 pipeline
Increase on DN150 pipeline flowmeter (left unused DN100 flowmeter with shurry pump to pelletizer, variable diameter installation carried out to pipeline,
Specific location scene determines), for conveying the phosphorus ammonium filtrate in phosphoric acid,diluted ageing tank.Other one still for conveying phosphoric acid,diluted.
Phosphorus ammonium filtrate is delivered to phosphoric acid concentrating device after being mixed on delivery pump outlet line with phosphoric acid,diluted and is concentrated.
The cement pit that former fluorine containing waste water is handled is transformed anti-corrosion, is used as and rinses pond, by filter-pressing device rushing originally
Washing basin installs agitating paddle, is used as ammonification slurry storage tank.
Calculating benchmark: in the test carried out according to the technique and scheme of the present invention, in conjunction in actual production, 66%MAP device
Production is practical, Fe2O3、Al2O3, MgO removal efficiency be respectively 96%, 97%, 70%, filtrate P2O5Yield 55% evaporates water 1.3t/
t NH3, ammonia loss 0.5%, ammonia consumes 0.3t/t P2O5, filtrate P2O55.6% is reduced, filter cake contains liquid 35%, filter press filtration flux
0.163m3/m2·h。
With 66m2On the basis of filter press ability, MaterialBalance Computation is carried out by ageing tank phosphoric acid,diluted analysis data, as a result such as
Following table:
Phosphoric acid,diluted ammoniation process reduces impurity content and is mixed in the high-quality Diammonium phosphate (DAP) of concentration production with phosphoric acid,diluted in the present invention: dilute
Clear liquid is obtained after sour ammonification filtrate and clarification phosphoric acid,diluted mixing, is not crystallized, mixed liquor is easier to be concentrated in vacuo, concentrate
After being cooled to room temperature, the sludge precipitating in deacidification is outer, and there are also a small amount of ammonium salt crystallizations to be precipitated, and it is higher to show as solid content.Therefore
Concentrate, which had better not cool down, when industrial production is aged clarification, multiplies heat and directly DAP is sent to produce.
The phosphate portion of purification is neutralized by ammonia, is matched in the diluted acid provided by technique center with pH (4.0-4.5) and diluted acid
Data, the phosphoric acid degree of neutralization into monoammonium phosphate device are that 0.15-0.2 leads to phosphorus while discharging part reaction heat in N-process
Sour diammonium tail gas washing liquid degree of neutralization increases, and system response heat is reduced, and may influence the control and presentation quality of product moisture, together
When influence tail wash washing effect.
The tail gas generated in diluted acid ammonifying process need to enter DAP device exhaust washing system, increase the negative of washing tail gas
Lotus may cause pelletizer positive pressure, also increase the ammonia content in tail gas, will lead to the raising of cleaning solution degree of neutralization, influences product
Presentation quality and vent gas washing system operation.
Water 1.3t/t NH is evaporated in phosphoric acid,diluted ammonifying process3, according to ammonification load, evaporation water about 2.0-2.5t/h, water
Divide and enter vent gas washing system, influence the water balance of DAP device, produces waste liquid outlet, lead to P2O5、NH3Loss.
According to the designed capacity of full automatic pressure filter, the filters pressing amount of ammonification slurry is estimated not to exceed 15m3/ h, filtrate produce
Raw amount is in 10m3Within/h, to match and be concentrated according to the technical solution of technique center, device capability mismatches.
The total nutrient that can be generated in phosphoric acid,diluted purification process reaches the filter residue of 55-MAP (butt), and multi-function device is needed to produce
It is consumed, therefore, when phosphoric acid,diluted purification system is run, multi-function device needs suitable compound fertilizer formula and carries out to filter residue
Consumption.Otherwise filter residue outlet will lead to ammonia, P2O5A large amount of losses.
Embodiment 2
A kind of technique of phosphoric acid,diluted demetalization ion, P2O5Mass concentration be 22% phosphoric acid,diluted from phosphoric acid,diluted clarifying tank bottom
Portion is pumped into ammoniation reactor, while being passed through liquefied ammonia and carrying out reaction 32min in pH=4.0~4.2, the phosphorus ammonium obtained after the reaction was completed
Slurry pH control is that 4.0-4.2 is sent into phosphor ammonium slurry storage tank, and for phosphor ammonium slurry after filter press filters pressing, phosphorus ammonium filtrate enters intermediate storage
Slot, and it is pumped to the storage of phosphoric acid,diluted ageing tank；
(2) the phosphorus ammonium filtrate after being aged is sent to enrichment facility after mixing with phosphoric acid,diluted and is concentrated, gelled acid to send to
Endpoint concentration 45%P2O5Enter monoammonium phosphate device afterwards and produces high-quality Diammonium phosphate (DAP)；The mass fraction of control phosphorus ammonium filtrate accounts for 25~
28%, mixed phosphoric acid MER are 0.06.
(3) filter residue after being aged send to multi-function device and produces compound fertilizer.
Claims (5)
1. a kind of technique of phosphoric acid,diluted demetalization ion, which comprises the steps of:
(1) phosphoric acid,diluted is pumped into ammoniation reactor from phosphoric acid,diluted defecator bottom, while being passed through liquefied ammonia and being reacted, after the reaction was completed
Obtained phosphor ammonium slurry is sent into phosphor ammonium slurry storage tank, and for phosphor ammonium slurry after filter press filters pressing, phosphorus ammonium filtrate enters hold-up vessel, and
It is pumped to the storage of phosphoric acid,diluted ageing tank；
(2) the phosphorus ammonium filtrate after being aged is sent to enrichment facility after mixing with phosphoric acid,diluted to be concentrated, and gelled acid send to phosphorus ammonium and fills
Set production Diammonium phosphate (DAP)；
(3) filter residue after being aged send to multi-function device and produces compound fertilizer.
2. the technique of phosphoric acid,diluted demetalization ion described in claim 1, which is characterized in that in phosphoric acid,diluted and liquefied ammonia reaction process
Slurry pH=4.0~4.5 are controlled, the aminating reaction time is 30min-50min, and phosphorus ammonium filtrate pH control is 4.0-4.5 after reaction,
The P that the phosphoric acid,diluted mass concentration is 20%~25%2O5。
3. the technique of phosphoric acid,diluted demetalization ion described in claim 1, which is characterized in that phosphorus ammonium filtrate mixes with phosphoric acid,diluted
Afterwards, the mass fraction for controlling phosphorus ammonium filtrate accounts for 25~30%, mixed phosphoric acid MER≤0.085.
4. the technique of phosphoric acid,diluted demetalization ion described in claim 1, which is characterized in that after phosphorus ammonium filtrate mixes with phosphoric acid,diluted
Striking point concentration 40-46% P2O5。
5. the technique of phosphoric acid,diluted demetalization ion described in claim 1, which is characterized in that the metal ion include Fe,
Al, Mg metal ion.
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| CN201811058373.9A CN109019545A (en) | 2018-09-11 | 2018-09-11 | A kind of technique of phosphoric acid,diluted demetalization ion |
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| CN201811058373.9A CN109019545A (en) | 2018-09-11 | 2018-09-11 | A kind of technique of phosphoric acid,diluted demetalization ion |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110526225A (en) * | 2019-09-29 | 2019-12-03 | 云南佳贝节能科技有限公司 | A kind for the treatment of process of phosphoric acid removing heavy metal |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1792778A (en) * | 2005-12-29 | 2006-06-28 | 叶树滋 | Process for preparing high purity phosphoric acid-ammonium by titanium dioxide waste acid |
| CN104261371A (en) * | 2014-09-01 | 2015-01-07 | 云南云天化国际化工有限公司 | Method for producing diammonium phosphate from high-impurity phosphorite |
| CN106672932A (en) * | 2017-01-10 | 2017-05-17 | 龙蟒大地农业有限公司 | Method for producing monoammonium phosphate by utilizing magnesium-free mother solution |
| CN107539971A (en) * | 2017-09-12 | 2018-01-05 | 甘肃瓮福化工有限责任公司 | A kind of production technology of MAP |
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2018
- 2018-09-11 CN CN201811058373.9A patent/CN109019545A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1792778A (en) * | 2005-12-29 | 2006-06-28 | 叶树滋 | Process for preparing high purity phosphoric acid-ammonium by titanium dioxide waste acid |
| CN104261371A (en) * | 2014-09-01 | 2015-01-07 | 云南云天化国际化工有限公司 | Method for producing diammonium phosphate from high-impurity phosphorite |
| CN106672932A (en) * | 2017-01-10 | 2017-05-17 | 龙蟒大地农业有限公司 | Method for producing monoammonium phosphate by utilizing magnesium-free mother solution |
| CN107539971A (en) * | 2017-09-12 | 2018-01-05 | 甘肃瓮福化工有限责任公司 | A kind of production technology of MAP |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110526225A (en) * | 2019-09-29 | 2019-12-03 | 云南佳贝节能科技有限公司 | A kind for the treatment of process of phosphoric acid removing heavy metal |
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Application publication date: 20181218 |