WO2005118470A1 - Procede de production d'acide phosphorique - Google Patents
Procede de production d'acide phosphorique Download PDFInfo
- Publication number
- WO2005118470A1 WO2005118470A1 PCT/EP2005/052495 EP2005052495W WO2005118470A1 WO 2005118470 A1 WO2005118470 A1 WO 2005118470A1 EP 2005052495 W EP2005052495 W EP 2005052495W WO 2005118470 A1 WO2005118470 A1 WO 2005118470A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- slurry
- phosphoric acid
- filter
- mixture
- filtration
- Prior art date
Links
Classifications
-
- 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
- C01B25/22—Preparation by reacting phosphate-containing material with an acid, e.g. wet process
- C01B25/222—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen
- C01B25/223—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen only one form of calcium sulfate being formed
- C01B25/225—Dihydrate process
-
- 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
- C01B25/22—Preparation by reacting phosphate-containing material with an acid, e.g. wet process
- C01B25/222—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen
- C01B25/223—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen only one form of calcium sulfate being formed
- C01B25/226—Hemihydrate process
Definitions
- Method for producing phosphoric acid The present invention relates to a method for producing phosphoric acid, comprising - forming a first aqueous slurry containing calcium sulphate dihydrate and phosphoric acid,
- 1,836,672 relates to a two-step process, namely a first step which involves the reaction of phosphate and sulfuric acid with simultaneous production of hemihydrate and concentrated phosphoric acid, the latter being then separated by a filtration operation, while, in a second stage, the hemihydrate, still soaked with phosphoric acid, is resuspended in a sulfophosphoric medium, under acidity and temperature conditions such as calcium recrystallizes from dihydrate.
- porridges can optionally contain calcium sulfate dihydrate or hemihydrate.
- the filter cake obtained therefore consists of superimposed layers of calcium sulfate dihydrate or hemihydrate without interpenetration of one layer into the other.
- the aim of this process is to increase the P 2 O 5 concentration of the phosphoric acid produced in the last of the reaction zones.
- This relatively complex and delicate process to master has the disadvantage of an uneconomic yield of the installation.
- calcium sulfate hemihydrate or dihydrate is always filtered separately.
- gypsum represents a by-product to be landfilled.
- heaping can only be done under well-defined conditions, in places that are sometimes far from production sites.
- the gypsum obtained carries with it large quantities of water which make it is difficult to handle and increases the cost of dry transport. In addition there is a risk of polluting groundwater at the place of discharge.
- the wet processes used in industry, which allow the production of concentrated phosphoric acid (more than 40% of P2O5), have long encountered the difficulties resulting from the simultaneous production of calcium sulfate hemihydrate and the high temperature: the working conditions lead to corrosion and incrustation phenomena resulting in additional production costs.
- the object of the present invention is to develop a process for the production of phosphoric acid which makes it possible to overcome the aforementioned drawbacks, while allowing the implementation of a technically simple installation or even an easy adaptation of an installation currently in service. This problem is solved according to the invention by a method as indicated at the beginning, this method comprising
- the method comprises, before filtration, a mixture of the first aqueous slurry and the second aqueous slurry and a supply of the filter with said mixture.
- This mixing can be done in a simple manner, for example by connecting the supply pipe of the filter to the outlet pipes of the tanks where the two slurries of the process according to the invention are produced.
- We may also further provide an intermediate mixer where the two slurries are mixed.
- the method according to the invention also provides for a simultaneous supply of the filter with said first slurry and said second slurry and a mixture of these two slurries in the filter itself.
- the aqueous slurries can be obtained by any suitable means. One can for example consider that one or the other or both come from a sulfuric attack of phosphate ores.
- the hemihydrate slurry is formed from part of the dihydrate slurry, for example by modifying the temperature and / or acidity conditions of this part drawn off from the dihydrate porridge.
- a modification only requires the mounting of a single additional tank provided at the outlet of the attack tank of an existing installation.
- the process then advantageously comprises a sulfuric attack on phosphate ore with the formation of said first aqueous slurry, a drawing off of part of said first aqueous slurry, and a treatment thereof giving rise to a conversion of said first aqueous slurry in said second aqueous slurry.
- This treatment can comprise, for example, the addition of sulfuric acid to said withdrawn part of the first aqueous slurry, or a heating thereof, for example by heating the tank or by injecting steam into the slurry, or both processes simultaneously.
- the dihydrate slurry is formed from part of the hemihydrate boil.
- hemihydrate porridge is a more acidic medium than dihydrate boil, that is, it contains a higher content of sulfuric acid.
- This installation comprises an attack tank 1 into which ground mineral phosphate is introduced in 2 and sulfuric acid in 3, as well as, in 4, the aqueous solution of phosphoric acid recycled from the process according to the invention .
- the attack conditions are applied in a known manner to obtain an aqueous slurry containing calcium sulphate dihydrate and phosphoric acid, which slurry is drawn off from tank 1 by the outlet conduit 5.
- a portion of this slurry withdrawn from tank 1 is withdrawn through the sampling conduit 6 and brought to a conversion tank 7.
- the slurry is treated so as to be converted into an aqueous slurry containing calcium sulfate hemihydrate and l 'Phosphoric acid.
- the treatment applied in this exemplary embodiment consists in introducing in 8 an additional sulfuric acid and / or in heating the tank and / or in injecting in 9 steam of water into the slurry. Any other suitable heat source can of course be used for this purpose. Under the effect of the increase in acidity and / or temperature, the dihydrate turns into hemihydrate. The remaining part of the slurry withdrawn from the tank 1 is, via the conduit 10, brought to a mixing step illustrated by the arrow 11. The slurry treated in the tank 7 is brought to this same mixing step by an outlet conduit 12.
- This mixing step can be carried out, as shown, using a common supply conduit into which the conduits 10 and 12 open, but also for example by means of a stirring tank into which open these conduits 10 and 12, and from which a mixture is discharged to the filter 13. It is also possible to envisage a simultaneous supply of the two slurries by the conduits 10 and 12 leading directly to the filter 13 where the mixing takes place.
- the filter 13 can be any suitable known filtration device, for example a band filter, a filter cell device arranged in a carousel, etc.
- the mixture of the two slurries is filtered in a first section of the filter, obtaining a filtrate at 14 which is the product of the process, that is to say an aqueous solution of phosphoric acid.
- the process illustrated comprises two stages of washing the cake, after filtration.
- the second washing is carried out using a washing liquid which is for example water, supplied with 15.
- the washing product obtained at 16 is recycled at 17 as washing liquid for the first washing step.
- the washing product obtained in 18, which comes from the first washing step, is an aqueous solution of phosphoric acid which can be recycled in 4 to the attack tank 1, via a recycling conduit. 19. If the filtered phosphoric acid obtained at the outlet pipe 14 has too high a residual sulfuric acid content, provision may be made to open this pipe 14 in a desulfation tank 20 provided with an agitator and supplied with 21 for example by a supplement of phosphate ore.
- the mixture of the two slurries contains calcium sulfate dihydrate and calcium sulfate hemihydrate in a weight ratio of 90/10 to 10/90, preferably 70/30 to 30/70. It is also possible to provide on the filter, upstream or downstream of the filtration of the mixture according to the invention, a supply of the filter with at least one additional aqueous slurry containing for example only dihydrate, only hemihydrate or a mixture of these, in particular in proportions different from those provided in the mixing step 1 1.
- the process according to the invention will now be described in more detail with the aid of exemplary embodiments given by way of illustration and not limiting.
- Example 1 Two series of 4 tests were carried out. In each series of tests, the slurries were fed to the filter in four different ways: 1. feeding a hemihydrate porridge (20% by weight) first, followed by a gypsum porridge (80% by weight)
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Luminescent Compositions (AREA)
- Fertilizers (AREA)
- Paper (AREA)
Abstract
Description
Claims
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
BRPI0510525-0A BRPI0510525A (pt) | 2004-06-01 | 2005-06-01 | processo de produção de ácido fosfórico |
EA200602217A EA010973B1 (ru) | 2004-06-01 | 2005-06-01 | Способ получения фосфорной кислоты |
CN2005800179148A CN1960941B (zh) | 2004-06-01 | 2005-06-01 | 生产磷酸的方法 |
EP05756810A EP1771378A1 (fr) | 2004-06-01 | 2005-06-01 | Procede de production d'acide phosphorique |
TNP2006000394A TNSN06394A1 (fr) | 2004-06-01 | 2006-11-30 | Procede de production d'acide phosphorique |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
BE2004/0273A BE1016065A3 (fr) | 2004-06-01 | 2004-06-01 | Procede de production d'acide phosphorique. |
BE2004/0273 | 2004-06-01 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2005118470A1 true WO2005118470A1 (fr) | 2005-12-15 |
Family
ID=34973657
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP2005/052495 WO2005118470A1 (fr) | 2004-06-01 | 2005-06-01 | Procede de production d'acide phosphorique |
Country Status (8)
Country | Link |
---|---|
EP (1) | EP1771378A1 (fr) |
CN (1) | CN1960941B (fr) |
BE (1) | BE1016065A3 (fr) |
BR (1) | BRPI0510525A (fr) |
EA (1) | EA010973B1 (fr) |
MA (1) | MA28704B1 (fr) |
TN (1) | TNSN06394A1 (fr) |
WO (1) | WO2005118470A1 (fr) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2011067321A1 (fr) | 2009-12-02 | 2011-06-09 | Prayon Technologies | Procede de production d'acide phosphorique |
WO2012163425A1 (fr) | 2011-06-01 | 2012-12-06 | Prayon Technologies | Procede de production d'acide phosphorique du type dihydrate/hemihydrate |
WO2019030403A1 (fr) | 2017-08-11 | 2019-02-14 | Prayon Technologies | Procede d'attaque acide d'une source phosphatee |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
RU2599525C1 (ru) * | 2015-04-23 | 2016-10-10 | Открытое акционерное общество "Научно-исследовательский институт по удобрениям и инсектофунгицидам имени профессора Я.В. Самойлова" (ОАО "НИУИФ") | Способ получения экстракционной фосфорной кислоты |
CN107840317B (zh) * | 2017-10-30 | 2019-12-03 | 安徽六国化工股份有限公司 | 一种一步法二水-半水湿法磷酸生产工艺 |
CN107840316B (zh) * | 2017-10-30 | 2019-07-19 | 安徽六国化工股份有限公司 | 一种二步法二水湿法磷酸生产工艺 |
Citations (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB1052986A (fr) * | 1962-06-29 | |||
GB313036A (en) | 1928-06-05 | 1929-07-04 | Kunstdunger Patent Verwertungs | Method of leaching raw phosphate |
US1836672A (en) | 1930-02-13 | 1931-12-15 | Kunstdunger Patent Verwertungs | Method of leaching phosphate rock |
BE660216A (fr) | 1964-02-27 | 1965-06-16 | ||
GB1007898A (en) | 1960-10-26 | 1965-10-22 | Nissan Chemical Ind Ltd | A process for the production of phosphoric acid and gypsum |
BE683739A (fr) | 1965-07-07 | 1967-01-06 | ||
US3632307A (en) * | 1969-04-09 | 1972-01-04 | Albatros Super Fosfaatfabrieke | Process for the preparation of phosphoric acid and gypsum from phosphate rock |
US3715191A (en) | 1970-07-13 | 1973-02-06 | Whiting Corp | Apparatus for making wet process phosphoric acid |
US3911079A (en) | 1971-03-23 | 1975-10-07 | Rhone Progil | Method of producing phosphoric acid and calcium sulphate |
US4220630A (en) | 1978-01-04 | 1980-09-02 | Occidental Petroleum Corporation | Hemihydrate type process for phosphoric acid manufacture using additive to improve filterability |
EP0027484A1 (fr) * | 1979-10-17 | 1981-04-29 | Societe Industrielle D'acide Phosphorique Et D'engrais S.I.A.P.E. | Dispositif pour améliorer la production d'acide phosphorique par voie humide |
EP0181029B1 (fr) | 1984-11-05 | 1991-06-12 | Prayon Développement Société anonyme | Procédé continu de préparation d'acide phosphorique et de sulfate de calcium |
US5084261A (en) * | 1989-06-22 | 1992-01-28 | Occidental Chemical Corporation | Recovery and utilization of gypstack leachate in hemihydrate phosphoric acid process |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3632304A (en) * | 1968-09-03 | 1972-01-04 | Universal Oil Prod Co | Catalytic oxidation of waste gas streams with fluidizable subdivided particles |
-
2004
- 2004-06-01 BE BE2004/0273A patent/BE1016065A3/fr active
-
2005
- 2005-06-01 CN CN2005800179148A patent/CN1960941B/zh not_active Expired - Fee Related
- 2005-06-01 BR BRPI0510525-0A patent/BRPI0510525A/pt not_active IP Right Cessation
- 2005-06-01 EA EA200602217A patent/EA010973B1/ru not_active IP Right Cessation
- 2005-06-01 EP EP05756810A patent/EP1771378A1/fr not_active Withdrawn
- 2005-06-01 WO PCT/EP2005/052495 patent/WO2005118470A1/fr active Application Filing
-
2006
- 2006-11-30 TN TNP2006000394A patent/TNSN06394A1/fr unknown
- 2006-12-29 MA MA29591A patent/MA28704B1/fr unknown
Patent Citations (15)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB313036A (en) | 1928-06-05 | 1929-07-04 | Kunstdunger Patent Verwertungs | Method of leaching raw phosphate |
US1902648A (en) | 1928-06-05 | 1933-03-21 | Kunstdunger Patentverwertungs | Method of leaching raw phosphate |
US1836672A (en) | 1930-02-13 | 1931-12-15 | Kunstdunger Patent Verwertungs | Method of leaching phosphate rock |
GB1007898A (en) | 1960-10-26 | 1965-10-22 | Nissan Chemical Ind Ltd | A process for the production of phosphoric acid and gypsum |
GB1052986A (fr) * | 1962-06-29 | |||
BE660216A (fr) | 1964-02-27 | 1965-06-16 | ||
BE683739A (fr) | 1965-07-07 | 1967-01-06 | ||
FR1485940A (fr) * | 1965-07-07 | 1967-06-23 | Prayon | Procédé pour la fabrication d'acide phosphorique et de sulfate de calcium hémihydrate par voie humide |
US3632307A (en) * | 1969-04-09 | 1972-01-04 | Albatros Super Fosfaatfabrieke | Process for the preparation of phosphoric acid and gypsum from phosphate rock |
US3715191A (en) | 1970-07-13 | 1973-02-06 | Whiting Corp | Apparatus for making wet process phosphoric acid |
US3911079A (en) | 1971-03-23 | 1975-10-07 | Rhone Progil | Method of producing phosphoric acid and calcium sulphate |
US4220630A (en) | 1978-01-04 | 1980-09-02 | Occidental Petroleum Corporation | Hemihydrate type process for phosphoric acid manufacture using additive to improve filterability |
EP0027484A1 (fr) * | 1979-10-17 | 1981-04-29 | Societe Industrielle D'acide Phosphorique Et D'engrais S.I.A.P.E. | Dispositif pour améliorer la production d'acide phosphorique par voie humide |
EP0181029B1 (fr) | 1984-11-05 | 1991-06-12 | Prayon Développement Société anonyme | Procédé continu de préparation d'acide phosphorique et de sulfate de calcium |
US5084261A (en) * | 1989-06-22 | 1992-01-28 | Occidental Chemical Corporation | Recovery and utilization of gypstack leachate in hemihydrate phosphoric acid process |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2011067321A1 (fr) | 2009-12-02 | 2011-06-09 | Prayon Technologies | Procede de production d'acide phosphorique |
US9255006B2 (en) | 2009-12-02 | 2016-02-09 | Prayon Technologies | Method for producing phosphoric acid |
WO2012163425A1 (fr) | 2011-06-01 | 2012-12-06 | Prayon Technologies | Procede de production d'acide phosphorique du type dihydrate/hemihydrate |
US9371230B2 (en) | 2011-06-01 | 2016-06-21 | Prayton Technologies | Dihydrate-hemihydrate process for producing phosphoric acid |
WO2019030403A1 (fr) | 2017-08-11 | 2019-02-14 | Prayon Technologies | Procede d'attaque acide d'une source phosphatee |
BE1025894A1 (fr) | 2017-08-11 | 2019-08-01 | Prayon Tech | Procede d’attaque acide d’une source phosphatee |
Also Published As
Publication number | Publication date |
---|---|
EA200602217A1 (ru) | 2007-04-27 |
TNSN06394A1 (fr) | 2008-02-22 |
CN1960941B (zh) | 2010-09-08 |
EP1771378A1 (fr) | 2007-04-11 |
CN1960941A (zh) | 2007-05-09 |
BRPI0510525A (pt) | 2007-10-30 |
BE1016065A3 (fr) | 2006-02-07 |
MA28704B1 (fr) | 2007-06-01 |
EA010973B1 (ru) | 2008-12-30 |
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