CN106744760A - The sedimentation agent and method of solids in rapid subsidence phosphoric acid by wet process - Google Patents
The sedimentation agent and method of solids in rapid subsidence phosphoric acid by wet process Download PDFInfo
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- CN106744760A CN106744760A CN201611100379.9A CN201611100379A CN106744760A CN 106744760 A CN106744760 A CN 106744760A CN 201611100379 A CN201611100379 A CN 201611100379A CN 106744760 A CN106744760 A CN 106744760A
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- phosphoric acid
- acid
- sedimentation agent
- fatty acid
- wet process
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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
- C01B25/235—Clarification; Stabilisation to prevent post-precipitation of dissolved impurities
Abstract
The sedimentation agent and method of solids in entitled rapid subsidence phosphoric acid by wet process of the invention.Belong to wet phosphoric acid purifying technical field.It is mainly the existing sedimentation agent of solution and is not suitable for concentration for 46 ~ 48%P2O5The problem of method phosphoric acid sedimentation.It is mainly characterized by：Sedimentation agent is made up of synthetic fatty acid that carbon chain lengths are 9~33 and salt of alpha sulfonated fatty acid；The COO of synthetic fatty acid and salt of alpha sulfonated fatty acid‑/SO3 2‑Match is 100：1〜1：100；It is the alkaline aqueous solution of mass concentration 10%；1. 1 ‰~10% sedimentation agent is added；2. stirred 55~70 minutes at a temperature of 47~53 DEG C；3. 10~40 minutes are stood；4. limpid bright phosphoric acid by wet process is filtered to obtain.Organic carbon granule clearance reaches 65~95%, F‑Clearance reach 55~92%, Fe3+Clearance reach 16.4~78%, Mg2+Clearance reach 14.5~66%, Al3+Clearance reach 19~55%, Ca2+Clearance reach 40~78%, Si4+Clearance reach 13~46%, the phosphoric acid by wet process for obtaining is limpid bright.
Description
Technical field
The invention belongs to wet phosphoric acid purifying technical field, and in particular to rapid subsidence solid in a kind of wet phosphoric acid purifying process
The excellent sedimentation agent and sedimentation method of thing.
Background technology
Phosphoric acid by wet process is substantially the mixing acid containing phosphoric acid, sulfuric acid and fluosilicic acid, and plurality of impurities is contained simultaneously（Such as Ca2+、
Mg2+、F-、Fe3+、Al3+、SO4 2-Plasma）.For in use, low-grade phosphate ore stone produce phosphoric acid by wet process technique, due to phosphorus
Organic matter in ore can be carbonized into Organic carbon when leaching；Substantial amounts of solids can be more produced after concentration, and with concentration
The reduction of phosphoric acid Temperature, can produce postprecipitation salt again；In addition abrasion of the phosphoric acid material to graphite evaporator in concentration process, makes wet
The quality of solids further increases in method phosphoric acid, acid solution is in black.Fortune of the presence of these solid sludge things to commercial phosphoric acid
Defeated, storage and subsequent production MAP, Diammonium phosphate (DAP) are all very unfavorable；Especially increase the refined difficulty of phosphoric acid.Cause
This, it is necessary to sludge is removed.
Traditional way is using the method for natural subsidence.After wet-process phosphoric acid concentration, by the natural subsidence in subsider,
Solids particles are allowed to sink naturally by gravity.This technique needs large-scale precipitation apparatus, the sedimentation time 15 days at most 30 days at least,
Its acid solution can only also settle out larger solid particle, and acid solution is still black, and the wt of amount containing stereoplasm>1%；Reduce production
Efficiency, improves production cost.
At present, in production practices, the most frequently used, simple, cheap method is to use chemical deposition method.With addition flocculant
By the disperse particles in phosphoric acid solution（Including the particulate in colloidal solution）Reunion settles down, then again using centrifugation,
The methods such as filtering are carried out separation of solid and liquid, to remove, reduce impurity therein（Or reclaim utility）, obtain peace and quiet liquid
Body（Clear liquid）.
Feng Licheng of Sichuan University in 2001 et al. have studied phosphoric acid material pulp flocculating setting optimize technique；Sichuan is big within 2004
Learn the small influence that have studied Flocculants on Sedimentation Characteristics of Phosphoric Acid Slurry such as beautiful of poplar；Their research concentrates on phosphoric acid,diluted
（18.5wt% ~ 30wt%P2O5）On sludge flocculating setting.Huang China of Central China Normal University in 2005 et al. have studied by nonionic
The multi-functional sedimentation agent of the part of flocculant-anion surfactant two composition processes the gelled acid of phosphoric acid by wet process, obtains liquid on earth
≤ 20% clarification phosphoric acid, the solid content≤0.5wt% of phosphoric acid clear liquid, fluorine removal efficiency >=84%.Hubei richness nation science and technology share in 2011
Left university of Co., Ltd et al. have studied by flocculant in non-ion type-coagulation-flocculation adsorbent-anion surfactant three
The multi-functional sedimentation agent of part composition processes the gelled acid of phosphoric acid by wet process, obtains the clarification phosphoric acid of liquid≤15% on earth.Wu Jie in 2013
Have studied the multi-functional sedimentation agent being made up of flocculant in non-ion type-part of anion surfactant-barium salt three and process wet method
The gelled acid of phosphoric acid, it is concentrated after obtain content >=85% of phosphoric acid.Hubei Xingfa Chemical Group Corp., Ltd. in 2013
Luo Baorui et al. have studied the sedimentation being made up of anionic flocculant-flocculant in non-ion type-part of adsorbent-defluorinating agent four
Agent processes the gelled acid of phosphoric acid by wet process.
The use of phosphoric acid by wet process sedimentation agent can substantially shorten the sedimentation time, improve settling efficiency, reduce storage tank quantity, section
About space, reduces production cost, simplifies production management program；Obtained phosphoric acid by wet process turbidity reduction can be made simultaneously, become clear
It is clear；Which part metal impurities ion Fe3+、Al3+、Ca2+、Mg2+、Si4+Etc. can be caught by the net of sedimentation agent, built bridge, rolled up sweep,
Charge neutrality etc. act on flco reunion, sedimentation be able to part remove, improve the quality of phosphoric acid by wet process；Reduce follow-up work
The use of the triviality and medicament of sequence, also reduces the refined difficulty of phosphoric acid, reduces the discharge of tailings；Be conducive to improving follow-up
The quality of product, reduction production cost.
The production of current phosphorous chemical industry, because phosphorus ore grade is not relatively high, the concentration of the concentrated wet-process phosphoric acid produced is
46~48%P2O5Left and right, viscosity is larger, and foreign ion is with cation such as Al3+、Fe3+、Ca2+、Mg2+、Si4+Etc. in the majority, flocculant is very
Hardly possible adsorbs sludge particles；Even if absorption, arch formation causes that sludge is very loose, causes bottom liquid too high.Therefore, these waddings
Solidifying agent shows as settling incomplete, bottom liquid excessive height, it is impossible to the phosphoric acid clarified, fouling in being used in concentration raw phosphoric acid sedimentation
Seriously；Settle the time for needing it is more long, it is necessary to storage tank quantity it is more, the space for occupying is larger, and production efficiency is low, produces
The concentrated wet-process phosphoric acid for arriving it is of low quality, increased subsequent technique treatment difficulty, have impact on the quality of downstream product.
The content of the invention
The purpose of the present invention is directed to the sedimentation of above-mentioned sedimentation agent performance in concentration raw phosphoric acid sedimentation not exclusively, and sludge is very
It is loose, bottom liquid excessive height, it is impossible to the phosphoric acid clarified, fouling serious problem during equipment long-play, there is provided
Plant the sedimentation agent of solids in rapid subsidence phosphoric acid by wet process.
The technical solution of sedimentation agent of the present invention is：The sedimentation agent of solids in a kind of rapid subsidence phosphoric acid by wet process, its
It is characterised by：The sedimentation agent is by aliphatic acid and α that carbon chain lengths are 9~33-Alpha-sulfonated fatty acid is constituted；Aliphatic acid and α-Sulfonate grease
The COO of fat acid-/SO3 2-Match is 100：1〜1：100；It is the alkaline aqueous solution of mass concentration 10%；
Concrete structure formula is：
In formula：N=6~30.
Aliphatic acid described in the technical solution of sedimentation agent of the present invention be natural acid, synthetic fatty acid or other
Esters；Sedimentation agent is obtained with raw material of fatty acid with sulfur trioxide Direct Sulfonation.
The technical solution of sedimentation method of the present invention is：One kind is according to solid in above-mentioned sedimentation agent rapid subsidence phosphoric acid by wet process
The method of body thing, it is characterised in that：1. toward P2O5Mass content be add in 24~48% raw phosphoric acids 1 ‰~10% sedimentation agent；
2. stirred 55~70 minutes at a temperature of 47~53 DEG C；3. 10~40 minutes are stood after stirring is finished；4. filter limpid bright
Phosphoric acid by wet process.
The aliphatic acid 1. described in step is natural acid, synthesis in the technical solution of sedimentation method of the present invention
Aliphatic acid or other esters；Sedimentation agent is obtained with raw material of fatty acid with sulfur trioxide Direct Sulfonation.
The present invention eliminates the electric charge of raw phosphoric acid using surfactant is added, and reduces the viscosity of raw phosphoric acid；Meanwhile, sedimentation
Agent can in acid condition generate the precipitation such as calcium salt, magnesium salts, allow sedimentation agent fully to adsorb sludge particles, reach the mesh of abundant sedimentation
's.
When the collocation of sedimentation agent and surfactant is selected, it is contemplated that raw phosphoric acid cationic such as Al3+、Fe3+、Ca2+、
Mg3+、Si4+Etc. in the majority, viscosity is big and flocculant and the mutual influence factor of surfactant, filter out carbon chain lengths for 9~
33 aliphatic acid and α-Alpha-sulfonated fatty acid.Aliphatic acid and α-The COO of alpha-sulfonated fatty acid-/SO3 2-Match is 100：1〜1：100, system
Into mass concentration be 10% alkaline aqueous solution as sedimentation agent.
Sedimentation agent addition in raw phosphoric acid is 1 ‰~the 10% of raw phosphoric acid volume.
The present invention has advantages below：（1）Substantially shorten the sedimentation time of phosphoric acid by wet process, even more than ten days contract by a few hours
It is short within 40 minutes so that dilute, the SPA quality produced is as clear as crystal, solves and settle needs in Wet-process Phosphoric Acid Production
Time it is more long, it is necessary to storage tank quantity it is more, the space for occupying is larger, the low problem of production efficiency；（2）Phosphoric acid clear liquid
Color is taken on a new look significantly, and between wt1-2%, present solid content is general in below wt0.05%, is subsequent production for originally solid content
MAP, Diammonium phosphate (DAP) provide high-quality raw material；（3）Effectively reduce F in phosphoric acid liquid-、Fe3+、Mg3+、Al3+、Ca2+、
Si4+Deng the content of cation, metal oxide and gypsum impurity major part are deposited in phosphoric acid sedimentation trench bottom, are discharged to reactive tank
In recycle, heater scale formation is also significantly reduced, and the effect of concentration preferably, greatlys save steam.
Specific embodiment
The present invention is described in detail with specific embodiment below.
Embodiment 1：Sedimentation agent is by synthetic fatty acid and α that carbon chain lengths are 33-Alpha-sulfonated fatty acid is constituted.Aliphatic acid and α-
The COO of alpha-sulfonated fatty acid-/SO3 2-Match is 100：1, be made mass concentration for 10% alkaline aqueous solution as sedimentation agent.
Toward 5000Kg/t（P2O5Meter）The sedimentation agent for adding 1 ‰ present invention to specify in 24% industrial dilute phosphoric acid liquid, at 50 DEG C
At a temperature of stir 60 minutes, stirring finish after stand 40 minutes, after testing organic carbon granule clearance reach 95%, F-Clearance
Reach 87%, Fe3+Clearance reach 37%, Mg2+Clearance reach 24%, Al3+Clearance reach 25%, Ca2+Clearance
Reach 70%, Si4+Clearance reach 13%, the phosphoric acid by wet process for obtaining is limpid bright.
Embodiment 2：Sedimentation agent is by synthetic fatty acid and α that carbon chain lengths are 9-Alpha-sulfonated fatty acid is constituted.Aliphatic acid and α-Sulphur
Change the COO of aliphatic acid-/SO3 2-Match is 10：1, be made mass concentration for 10% aqueous solution as sedimentation agent.
Toward 10000Kg/t（P2O5Meter）The sedimentation agent for adding 10% present invention to specify in 26% industrial dilute phosphoric acid liquid, at 53 DEG C
At a temperature of stir 55 minutes, stirring finish after stand 10 minutes, after testing organic carbon granule clearance reach 90%, F-Clearance
Reach 92%, Fe3+Clearance reach 78%, Mg2+Clearance reach 34%, Al3+Clearance reach 26%, Ca2+Clearance
Reach 67%, Si4+Clearance reach 46%, the phosphoric acid by wet process for obtaining is limpid bright.
Embodiment 3：Sedimentation agent is by synthetic fatty acid and α that carbon chain lengths are 33-Alpha-sulfonated fatty acid is constituted.Aliphatic acid and α-
The COO of alpha-sulfonated fatty acid-/SO3 2-Match is 1：100, be made mass concentration for 10% alkaline aqueous solution as sedimentation agent.
Toward 5000Kg/t（P2O5Meter）The sedimentation agent for adding 1% present invention to specify in 24% industrial dilute phosphoric acid liquid, in 47 DEG C of temperature
The lower stirring of degree 70 minutes, stirring stands 40 minutes after finishing, and organic carbon granule clearance reaches 95%, F after testing-Clearance reach
To 90%, Fe3+Clearance reach 53%, Mg2+Clearance reach 66%, Al3+Clearance reach 46%, Ca2+Clearance reach
To 78%, Si4+Clearance reach 43%, the phosphoric acid by wet process for obtaining is limpid bright.
Embodiment 4：Sedimentation agent is by synthetic fatty acid and α that carbon chain lengths are 33-Alpha-sulfonated fatty acid is constituted.Aliphatic acid and α-
The COO of alpha-sulfonated fatty acid-/SO3 2-Match is 100：1, be made mass concentration for 10% alkaline aqueous solution as sedimentation agent.
Toward 3600Kg/t（P2O5Meter）The sedimentation agent for adding 1% present invention to specify in 46% industrial SPA liquid, in 49 DEG C of temperature
The lower stirring of degree 62 minutes, stirring stands 35 minutes after finishing, and organic carbon granule clearance reaches 95%, F after testing-Clearance reach
To 90%, Fe3+Clearance reach 51%, Mg2+Clearance reach 35%, Al3+Clearance reach 19%, Ca2+Clearance reach
To 68%, Si4+Clearance reach 33%, the phosphoric acid by wet process for obtaining is limpid bright.
Embodiment 5：Sedimentation agent is by synthetic fatty acid and α that carbon chain lengths are 33-Alpha-sulfonated fatty acid is constituted.Aliphatic acid and α-
The COO of alpha-sulfonated fatty acid-/SO3 2-Match is 100：1, be made mass concentration for 10% alkaline aqueous solution as sedimentation agent.
Toward 2000Kg/t（P2O5Meter）The sedimentation agent for adding 1 ‰ present invention to specify in 48% industrial dilute phosphoric acid liquid, at 52 DEG C
At a temperature of stir 60 minutes, stirring finish after stand 30 minutes, after testing organic carbon granule clearance reach 69%, F-Clearance
Reach 55%, Fe3+Clearance reach 16.4%, Mg2+Clearance reach 14.5%, Al3+Clearance reach 33.4%, Ca2+'s
Clearance reaches 50%, Si4+Clearance reach 14.8%, the phosphoric acid by wet process for obtaining is limpid bright.
Embodiment 6：Sedimentation agent is by synthetic fatty acid and α that carbon chain lengths are 33-Alpha-sulfonated fatty acid is constituted.Aliphatic acid and α-
The COO of alpha-sulfonated fatty acid-/SO3 2-Match is 1：1, be made mass concentration for 10% alkaline aqueous solution as sedimentation agent.
Toward 5000Kg/t（P2O5Meter）The sedimentation agent for adding 10% present invention to specify in 24% industrial dilute phosphoric acid liquid, at 48 DEG C
At a temperature of stir 65 minutes, stirring finish after stand 38 minutes, after testing organic carbon granule clearance reach 95%, F-Clearance
Reach 87%, Fe3+Clearance reach 43%, Mg2+Clearance reach 54%, Al3+Clearance reach 35%, Ca2+Clearance
Reach 74%, Si4+Clearance reach 33%, the phosphoric acid by wet process for obtaining is limpid bright.
Embodiment 7：Sedimentation agent is by synthetic fatty acid and α that carbon chain lengths are 33-Alpha-sulfonated fatty acid is constituted.Aliphatic acid and α-
The COO of alpha-sulfonated fatty acid-/SO3 2-Match is 1：10, be made mass concentration for 10% alkaline aqueous solution as sedimentation agent.
Toward 3000Kg/t（P2O5Meter）The sedimentation agent for adding 1 ‰ present invention to specify in 24% industrial dilute phosphoric acid liquid, at 48 DEG C
At a temperature of stir 65 minutes, stirring finish after stand 37 minutes, after testing organic carbon granule clearance reach 95%, F-Clearance
Reach 87%, Fe3+Clearance reach 37%, Mg2+Clearance reach 44%, Al3+Clearance reach 55%, Ca2+Clearance
Reach 70%, Si4+Clearance reach 33%, the phosphoric acid by wet process for obtaining is limpid bright.
Embodiment 8：Sedimentation agent is by synthetic fatty acid and α that carbon chain lengths are 17-Alpha-sulfonated fatty acid is constituted.Aliphatic acid and α-
The COO of alpha-sulfonated fatty acid-/SO3 2-Match is 10：1, be made mass concentration for 10% alkaline aqueous solution as sedimentation agent.
Toward 1000Kg/t（P2O5Meter）The sedimentation agent for adding 1% present invention to specify in 48% industrial dilute phosphoric acid liquid, in 49 DEG C of temperature
The lower stirring of degree 63 minutes, stirring stands 39 minutes after finishing, and organic carbon granule clearance reaches 90%, F after testing-Clearance reach
To 87%, Fe3+Clearance reach 37%, Mg2+Clearance reach 64%, Al3+Clearance reach 35%, Ca2+Clearance reach
To 70%, Si4+Clearance reach 23%, the phosphoric acid by wet process for obtaining is limpid bright.
Embodiment 9：Sedimentation agent is by synthetic fatty acid and α that carbon chain lengths are 9-Alpha-sulfonated fatty acid is constituted.Aliphatic acid and α-Sulphur
Change the COO of aliphatic acid-/SO3 2-Match is 10：1, be made mass concentration for 10% alkaline aqueous solution as sedimentation agent.
Toward 5000Kg/t（P2O5Meter）The sedimentation agent for adding 10% present invention to specify in 24% industrial dilute phosphoric acid liquid, at 50 DEG C
At a temperature of stir 58 minutes, stirring finish after stand 40 minutes, after testing organic carbon granule clearance reach 75%, F-Clearance
Reach 57%, Fe3+Clearance reach 37%, Mg2+Clearance reach 44%, Al3+Clearance reach 15%, Ca2+Clearance
Reach 70%, Si4+Clearance reach 33%, the phosphoric acid by wet process for obtaining is limpid bright.
Embodiment 10：Sedimentation agent is by synthetic fatty acid and α that carbon chain lengths are 9-Alpha-sulfonated fatty acid is constituted.Aliphatic acid and α-
The COO of alpha-sulfonated fatty acid-/SO3 2-Match is 1：100, be made mass concentration for 10% alkaline aqueous solution as sedimentation agent.
Toward 1000Kg/t（P2O5Meter）The sedimentation agent for adding 1 ‰ present invention to specify in 24% industrial dilute phosphoric acid liquid, at 47 DEG C
At a temperature of stir 63 minutes, stirring finish after stand 38 minutes, after testing organic carbon granule clearance reach 65%, F-Clearance
Reach 57%, Fe3+Clearance reach 37%, Mg2+Clearance reach 24%, Al3+Clearance reach 25%, Ca2+Clearance
Reach 40%, Si4+Clearance reach 23%, the phosphoric acid by wet process for obtaining is limpid bright.
Embodiment 11：Sedimentation agent is by synthetic fatty acid and α that carbon chain lengths are 24-Alpha-sulfonated fatty acid is constituted.Aliphatic acid and α-
The COO of alpha-sulfonated fatty acid-/SO3 2-Match is 1：1, be made mass concentration for 10% alkaline aqueous solution as sedimentation agent.
Toward 1000Kg/t（P2O5Meter）The sedimentation agent for adding 1% present invention to specify in 48% industrial dilute phosphoric acid liquid, in 51 DEG C of temperature
The lower stirring of degree 59 minutes, stirring stands 36 minutes after finishing, and organic carbon granule clearance reaches 90%, F after testing-Clearance reach
To 77%, Fe3+Clearance reach 47%, Mg2+Clearance reach 64%, Al3+Clearance reach 45%, Ca2+Clearance reach
To 76%, Si4+Clearance reach 33%, the phosphoric acid by wet process for obtaining is limpid bright.
Embodiment 12：Sedimentation agent is by synthetic fatty acid and α that carbon chain lengths are 14-Alpha-sulfonated fatty acid is constituted.Aliphatic acid and α-
The COO of alpha-sulfonated fatty acid-/SO3 2-Match is 1：1, be made mass concentration for 10% alkaline aqueous solution as sedimentation agent.
Toward 3000Kg/t（P2O5Meter）The sedimentation agent for adding 1% present invention to specify in 48% industrial dilute phosphoric acid liquid, in 51 DEG C of temperature
The lower stirring of degree 59 minutes, stirring stands 39 minutes after finishing, and organic carbon granule clearance reaches 88%, F after testing-Clearance reach
To 57%, Fe3+Clearance reach 47%, Mg2+Clearance reach 60%, Al3+Clearance reach 48%, Ca2+Clearance reach
To 79%, Si4+Clearance reach 33%, the phosphoric acid by wet process for obtaining is limpid bright.
Claims (4)
1. in a kind of rapid subsidence phosphoric acid by wet process solids sedimentation agent, it is characterised in that：The sedimentation agent by carbon chain lengths be 9~
33 aliphatic acid and α-alpha-sulfonated fatty acid composition；The COO of aliphatic acid and α-alpha-sulfonated fatty acid-/SO3 2-Match is 100：1〜1：
100；It is the alkaline aqueous solution of mass concentration 10%；
Concrete structure formula is：
In formula：N=6~30.
2. in a kind of rapid subsidence phosphoric acid by wet process according to claim 1 solids sedimentation agent, it is characterised in that：It is described
Aliphatic acid be natural acid, synthetic fatty acid or other esters；Sedimentation agent with raw material of fatty acid, with the direct sulphur of sulfur trioxide
Change and be obtained.
3. in a kind of sedimentation agent rapid subsidence phosphoric acid by wet process according to claim 1 solids method, it is characterised in that：
1. toward P2O5Mass content be add in 24~48% raw phosphoric acids 1 ‰~10% sedimentation agent；2. stirred at a temperature of 47~53 DEG C
55~70 minutes；3. 10~40 minutes are stood after stirring is finished；4. limpid bright phosphoric acid by wet process is filtered to obtain.
4. in rapid subsidence phosphoric acid by wet process according to claim 3 solids method, it is characterised in that：1. in step
Described aliphatic acid is natural acid, synthetic fatty acid or other esters；Sedimentation agent is straight with sulfur trioxide with raw material of fatty acid
Connect sulfonation and be obtained.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114671419A (en) * | 2022-04-06 | 2022-06-28 | 武汉强盛科技有限公司 | Settling agent and method for rapidly reducing solid content of wet-process phosphoric acid |
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| CN114671419B (en) * | 2022-04-06 | 2024-04-12 | 武汉强盛科技有限公司 | Settling agent and method for rapidly reducing solid content of wet-process phosphoric acid |
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Application publication date: 20170531 |