EP0463905A1 - Process for separating silicon compounds from pickling baths and apparatus therefor - Google Patents
Process for separating silicon compounds from pickling baths and apparatus therefor Download PDFInfo
- Publication number
- EP0463905A1 EP0463905A1 EP91401525A EP91401525A EP0463905A1 EP 0463905 A1 EP0463905 A1 EP 0463905A1 EP 91401525 A EP91401525 A EP 91401525A EP 91401525 A EP91401525 A EP 91401525A EP 0463905 A1 EP0463905 A1 EP 0463905A1
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- EP
- European Patent Office
- Prior art keywords
- pickling bath
- pickling
- silicic compounds
- bath
- compounds
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000005554 pickling Methods 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 25
- 150000003377 silicon compounds Chemical class 0.000 title abstract description 8
- -1 iron ions Chemical class 0.000 claims abstract description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052742 iron Inorganic materials 0.000 claims abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 7
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 6
- 239000010959 steel Substances 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 150000001875 compounds Chemical class 0.000 claims description 25
- 238000001816 cooling Methods 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 11
- 238000005119 centrifugation Methods 0.000 claims description 6
- 238000009434 installation Methods 0.000 claims description 6
- 238000003303 reheating Methods 0.000 claims description 6
- 230000001172 regenerating effect Effects 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000010908 decantation Methods 0.000 claims description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 13
- 235000013980 iron oxide Nutrition 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 239000000377 silicon dioxide Substances 0.000 description 8
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 5
- 239000006096 absorbing agent Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000009616 inductively coupled plasma Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical class Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/36—Regeneration of waste pickling liquors
-
- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S423/00—Chemistry of inorganic compounds
- Y10S423/01—Waste acid containing iron
Definitions
- EP-0 141 034 discloses a process for separating a silicic compound from a spent pickling bath for steels.
- the spent pickling bath passes through a filter made of a material adsorbing the silica compound.
- Such a method has the drawback of requiring an operation for regenerating the adsorbent materials constituting the filter. In fact, during its use, the adsorbent filter becomes clogged and the flow rate and the volume of the pickling bath treated decreases progressively.
- pickling baths after having been previously concentrated are thermally decomposed by known methods and are in particular calcined in an oven of the RUTHNER type, which makes it possible to recover iron oxides, essentially in Fe2O3 form.
- the sufficiently pure iron oxides can be used as colorants, for example in paints and cosmetic products, or as excipients in the pharmaceutical industry. They are also used in the manufacture of magnetic components or still in the manufacture of cements to improve their mechanical characteristics.
- the silica content of the iron oxides currently recovered from the pickling baths is at least 350 ppm, while it would be desirable to lower it below 100 ppm for the applications mentioned above.
- the invention also relates to an installation comprising means for regenerating the pickling bath containing iron ions and silicic compounds, characterized in that the regenerating means further comprise at least one controlled cooling tank for the pickling bath and for reheating the latter and at least one device for separating the precipitated silica compound (s) from the pickling bath, the separation device advantageously consisting of a centrifugation device and / or a filtration device comprising filters of lower porosity or equal to 20 ⁇ m.
- FIG. 1 represents a diagram of an installation for pickling steel sheets.
- the installation comprises a pickling unit 1 at the outlet of which the pickling bath containing water, hydrochloric acid, iron chlorides and one or more silicic compounds is depleted in acid and enriched in iron.
- the bath temperature is around 90 ° C, it contains 30 to 60 g / l of hydrochloric acid and 90 to 140 g / l of iron ions, and optionally a compound preventing attack of the substrate.
- the spent pickling bath is then directed to an evaporator 2 to be concentrated there.
- the evaporator 2 consists of a liquid-gas exchanger supplied by hot gases leaving a device thermal 3 via a cyclone 4.
- the evaporator 2 makes it possible to preheat the bath while concentrating it by evaporation of the water contained in it.
- the concentrated spent bath recovered at the outlet of the evaporator 2 is directed to cooling and reheating tanks 5 and 6, where it is cooled to a temperature equal to or less than 60 ° C. preferably with a cooling rate about 2 ° C / min.
- the pickling bath is then allowed to cool for a period of at least 2 hours, which makes it possible to create favorable conditions for the silicic compounds to crystallize in the form of relatively large particles.
- the bath is heated so that the dissolution, in particular of the iron chloride, is sufficient and to obtain a viscosity of the bath allowing separation, for example by filtration of the silicic compound (s).
- the rate of reheating is not critical and can vary from a few minutes to several hours.
- the pickling bath is advantageously centrifuged and / or filtered on the centrifugation and / or automatic filtration unit 7 which makes it possible to collect the precipitated silicic compound (s) and not redissolved.
- the pickling bath depleted in silicic compounds is then directed to the upper part of the thermal device 3 where it is treated to obtain iron oxide. Iron oxide is collected at the base of the thermal device 3.
- the thermal device 3 known for implementing, for example, the RUTHNER process, the vapors of water and of acid produced containing a residual quantity of iron oxide are sent into a cyclone 4 which separates the iron oxide. The residual iron oxide thus separated is reintroduced into the thermal device 3.
- the hot gases taken off at the head of cyclone 4 are used for the operation of the evaporator 2.
- the hot gases essentially comprising water vapor and hydrochloric acid pass through an absorber 8 supplied with water in its upper part by water coming from the rinsing unit 9 used for rinsing the substrates leaving the pickling unit 1.
- the acid-depleted vapors exiting at the upper part of the absorber 8 are directed to a smoke washing device 10 supplied with water by an additional water 11.
- the smoke washing water is added to the supplying water the absorber 8 from the rinsing unit 9.
- a regenerated bath is collected containing a hydrochloric acid solution which can again be used for a second cycle of pickling and regeneration.
- the process and the device according to the invention for the substantial elimination of the silicic compounds from the pickling baths are easily transposable in an industrial environment and make it possible to obtain iron oxide whose silica content is less than 100 ppm.
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
Description
La présente invention concerne un procédé de séparation des composés siliciques des bains de décapage contenant des ions fer et des composés siliciques ainsi qu'un dispositif pour la mise en oeuvre du procédé.The present invention relates to a process for the separation of silicic compounds from pickling baths containing iron ions and silicic compounds as well as to a device for carrying out the process.
Il est connu de la demande EP-0 141 034 un procédé pour séparer un composé silicique d'un bain usé de décapage des aciers.EP-0 141 034 discloses a process for separating a silicic compound from a spent pickling bath for steels.
Dans ce procédé, le bain de décapage usé traverse un filtre constitué d'un matériau adsorbant le composé silicique.In this process, the spent pickling bath passes through a filter made of a material adsorbing the silica compound.
Un tel procédé à l'inconvénient de nécessiter une opération de régénération des matériaux adsorbants constituant le filtre. En effet, au cours de son utilisation, le filtre adsorbant s'obstrue et le débit et le volume du bain de décapage traité diminue progressivement.Such a method has the drawback of requiring an operation for regenerating the adsorbent materials constituting the filter. In fact, during its use, the adsorbent filter becomes clogged and the flow rate and the volume of the pickling bath treated decreases progressively.
Les bains de décapage actuellement utilisés pour le décapage de substrats en acier contiennent des ions fer, essentiellement sous forme d'ions ferreux, ainsi qu'une certaine proportion de composés siliciques formés à partir de l'élément silicium provenant du substrat.The pickling baths currently used for pickling steel substrates contain iron ions, essentially in the form of ferrous ions, as well as a certain proportion of silicic compounds formed from the silicon element coming from the substrate.
Ces bains de décapage après avoir été préalablement concentrés sont décomposés par voie thermique par des méthodes connues et sont notamment calcinés dans un four de type RUTHNER, ce qui permet de récupérer des oxydes de fer, essentiellement sous forme Fe₂O₃.These pickling baths after having been previously concentrated are thermally decomposed by known methods and are in particular calcined in an oven of the RUTHNER type, which makes it possible to recover iron oxides, essentially in Fe₂O₃ form.
Les oxydes de fer, suffisamment purs peuvent être utilisés comme colorants, par exemple dans les peintures et produits cosmétiques, ou comme excipients dans l'industrie pharmaceutique. Ils entrent également dans la fabrication de composants magnétiques ou encore dans la fabrication de ciments pour améliorer leurs caractéristiques mécaniques.The sufficiently pure iron oxides can be used as colorants, for example in paints and cosmetic products, or as excipients in the pharmaceutical industry. They are also used in the manufacture of magnetic components or still in the manufacture of cements to improve their mechanical characteristics.
La teneur en silice des oxydes de fer actuellement récupérés à partir des bains de décapage est au moins de 350 ppm, alors qu'il serait souhaitable d'abaisser celle-ci en-dessous de 100 ppm pour les applications mentionnées ci-dessus.The silica content of the iron oxides currently recovered from the pickling baths is at least 350 ppm, while it would be desirable to lower it below 100 ppm for the applications mentioned above.
Le but de la présente invention est de proposer un procédé permettant d'augmenter la pureté des oxydes de fer en abaissant leur teneur en composés siliciques résiduels.The object of the present invention is to provide a process for increasing the purity of iron oxides by lowering their content of residual silicic compounds.
L'invention a ainsi pour objet un procédé de séparation de composés siliciques des bains de décapage de substrats en acier contenant des ion fer et des composés du silicium, consistant en les étapes suivantes :
- a) on refroidit de manière contrôlée un bain de décapage usé concentré, à une température inférieure ou égale à 60°C, de manière à précipiter les composés du silicium,
- b) on laisse refroidir pendant au moins 2 heures le bain de décapage,
- c) on réchauffe le bain de décapage,
- d) on sépare les composés du silicium précipités du bain de décapage.
- a) a concentrated spent pickling bath is cooled in a controlled manner, to a temperature less than or equal to 60 ° C., so as to precipitate the silicon compounds,
- b) the pickling bath is allowed to cool for at least 2 hours,
- c) heating the pickling bath,
- d) separating the precipitated silicon compounds from the pickling bath.
Les autres caractéristiques avantageuses de l'invention sont :
- la vitesse de refroidissement contrôlé est comprise entre 0,2 et 4°C/mn, et est de préférence d'environ 2°C/mn,
- la température de refroidissement du bain de décapage est de préférence comprise entre 20 et 40°C,
- on réchauffe le bain de décapage à une température d'environ 80°C,
- les composés siliciques précipités sont séparés du bain de décapage par tout moyen approprié notamment par décantation, centrifugation et/ou filtration. Dans le cas d'une filtration, celle-ci est effectuée avantageusement sur des filtres ayant une porosité inférieure ou égale à 20 µm.
- the controlled cooling rate is between 0.2 and 4 ° C / min, and is preferably around 2 ° C / min,
- the cooling temperature of the pickling bath is preferably between 20 and 40 ° C,
- the pickling bath is heated to a temperature of around 80 ° C.,
- the precipitated silicic compounds are separated from the pickling bath by any suitable means, in particular by decantation, centrifugation and / or filtration. In the case of filtration, this is advantageously carried out on filters having a porosity less than or equal to 20 μm.
L'invention a également pour objet une installation comprenant des moyens pour la régénération du bain de décapage contenant des ions fer et des composés siliciques caractérisée en ce que les moyens de régénération comprennent en outre au moins un bac de refroidissement contrôlé du bain de décapage et de réchauffage de celui-ci et au moins un dispositif de séparation du ou des composés siliciques précipités du bain de décapage, le dispositif de séparation consistant avantageusement en un dispositif de centrifugation et/ou un dispositif de filtration comportant des filtres d'une porosité inférieure ou égale à 20 µm.The invention also relates to an installation comprising means for regenerating the pickling bath containing iron ions and silicic compounds, characterized in that the regenerating means further comprise at least one controlled cooling tank for the pickling bath and for reheating the latter and at least one device for separating the precipitated silica compound (s) from the pickling bath, the separation device advantageously consisting of a centrifugation device and / or a filtration device comprising filters of lower porosity or equal to 20 µm.
Le procédé et l'installation de l'invention sont décrits plus en détail ci-après en se référant à la fig. 1 qui représente un schéma d'une installation de décapage de tôles d'acier.The method and the installation of the invention are described in more detail below with reference to FIG. 1 which represents a diagram of an installation for pickling steel sheets.
L' installation comprend une unité de décapage 1 à la sortie de laquelle le bain de décapage contenant de l'eau, de l'acide chlorhydrique, des chlorures de fer et un ou plusieurs composés siliciques est appauvri en acide et enrichi en fer. La température du bain est d'environ 90°C, il contient de 30 à 60 g/l d'acide chlorhydrique et 90 à 140 g/l d'ions fer, et éventuellement un composé évitant l'attaque du substrat. Le bain usé de décapage est ensuite dirigé vers un évaporateur 2 pour y être concentré. L'évaporateur 2 est constitué d'un échangeur liquide-gaz alimenté par des gaz chauds sortant d'un dispositif thermique 3 par l'intermédiaire d'un cyclone 4.The installation comprises a pickling unit 1 at the outlet of which the pickling bath containing water, hydrochloric acid, iron chlorides and one or more silicic compounds is depleted in acid and enriched in iron. The bath temperature is around 90 ° C, it contains 30 to 60 g / l of hydrochloric acid and 90 to 140 g / l of iron ions, and optionally a compound preventing attack of the substrate. The spent pickling bath is then directed to an evaporator 2 to be concentrated there. The evaporator 2 consists of a liquid-gas exchanger supplied by hot gases leaving a device thermal 3 via a cyclone 4.
L'évaporateur 2 permet de préchauffer le bain tout en le concentrant par évaporation de l'eau contenue dans celui-ci.The evaporator 2 makes it possible to preheat the bath while concentrating it by evaporation of the water contained in it.
Le bain usé concentré récupéré à la sortie de l'évaporateur 2 est dirigé vers des bacs de refroidissement et de réchauffage 5 et 6, où il est refroidi jusqu'à une température égale ou inférieure à 60°C de préférence avec une vitesse de refroidissement d'environ 2°C/mn. On laisse ensuite refroidir le bain de décapage pendant une durée d'au moins 2 heures, ce qui permet de créer des conditions favorables pour que les composés siliciques cristallisent sous forme de particules relativement grosses.The concentrated spent bath recovered at the outlet of the evaporator 2 is directed to cooling and reheating
Ensuite, le bain est réchauffé pour que la dissolution notamment du chlorure de fer soit suffisante et pour obtenir une viscosité du bain permettant une séparation, par exemple par filtration du ou des composés siliciques.Then, the bath is heated so that the dissolution, in particular of the iron chloride, is sufficient and to obtain a viscosity of the bath allowing separation, for example by filtration of the silicic compound (s).
La vitesse de réchauffage n'est pas déterminante et peut varier de quelques minutes à plusieurs heures.The rate of reheating is not critical and can vary from a few minutes to several hours.
A la sortie des bacs de refroidissement et de réchauffage 5 et 6, le bain de décapage est avantageusement centrifugé et/ou filtré sur l'unité de centrifugation et/ou de filtration automatique 7 ce qui permet de recueillir le ou les composés siliciques précipités et non redissous.At the outlet of the cooling and reheating
Le bain de décapage appauvri en composés siliciques est alors dirigé vers la partie haute du dispositif thermique 3 où il est traité pour obtenir l'oxyde de fer. L'oxyde de fer est recueilli à la base du dispositif thermique 3.The pickling bath depleted in silicic compounds is then directed to the upper part of the
Dans le dispositif thermique 3 connu pour la mise en oeuvre par exemple du procédé RUTHNER, les vapeurs d'eau et d'acide produites contenant une quantité résiduelle d'oxyde de fer sont envoyées dans un cyclone 4 qui sépare l'oxyde de fer. L'oxyde de fer résiduel ainsi séparé est réintroduit dans le dispositif thermique 3.In the
Les gaz chauds prélevés en tête du cyclone 4 sont utilisés pour le fonctionnement de l'évaporateur 2.The hot gases taken off at the head of cyclone 4 are used for the operation of the evaporator 2.
A la sortie de l'évaporateur 2, les gaz chauds comprenant essentiellement de la vapeur d'eau et de l'acide chlorhydrique passent dans un absorbeur 8 alimenté en eau dans sa partie supérieure par de l'eau provenant de l'unité de rinçage 9 servant au rinçage des substrats qui sortent de l'unité de décapage 1.At the outlet of the evaporator 2, the hot gases essentially comprising water vapor and hydrochloric acid pass through an absorber 8 supplied with water in its upper part by water coming from the
Les vapeurs appauvries en acide sortant à la partie supérieure de l'absorbeur 8 sont dirigées vers un dispositif de lavage de fumées 10 alimenté en eau par un appoint d'eau 11. L'eau de lavage de fumée est ajoutée à l'eau alimentant l'absorbeur 8 à partir de l'unité de rinçage 9.The acid-depleted vapors exiting at the upper part of the absorber 8 are directed to a
A la partie inférieure de l'absorbeur 8, on recueille un bain régénéré contenant une solution d'acide chlorhydrique qui peut à nouveau être utilisée pour un secondcycle de décapage et de régénération.At the bottom of the absorber 8, a regenerated bath is collected containing a hydrochloric acid solution which can again be used for a second cycle of pickling and regeneration.
On donnera ci-après les résultats d'essais réalisés sur plusieurs bains de décapage en mettant en oeuvre le procédé selon l'invention qui a consisté à refroidir des bains de décapage contenant des ions fer et des composés siliciques de la température d'environ 80°C à une température d'environ 40°C avec une vitesse de refroidissement d'environ 2°C/mn, à laisser refroidir les bains de décapage pendant une durée d'environ 3 heures, à réchauffer les bains à 80°C, puis à séparer le ou les composés siliciques précipités des bains de décapage par filtration sur des filtres de porosité variable.The following will give the results of tests carried out on several pickling baths using the method according to the invention which consisted in cooling pickling baths containing iron ions and silicic compounds of the temperature of about 80 ° C at a temperature of about 40 ° C with a cooling rate of about 2 ° C / min, to allow to cool pickling baths for a period of approximately 3 hours, heating the baths to 80 ° C., then separating the precipitated silica compound (s) from the pickling baths by filtration on filters of variable porosity.
L'efficacité du procédé de l'invention est contrôlée par dosage du silicium ou de la silice selon les méthodes suivantes :
- méthode gravimétrique pour mesurer la quantité de silice retenue par les filtres
- méthode d'absorption atomique pour mesurer la quantité de silicium contenue dans le filtrat
- par ICP (Plasma à couplage inductif) pour mesurer la quantité de silicium dans les oxydes de fer obtenus par évaporation du bain de décapage.
- gravimetric method to measure the quantity of silica retained by the filters
- atomic absorption method to measure the amount of silicon in the filtrate
- by ICP (inductively coupled plasma) to measure the quantity of silicon in the iron oxides obtained by evaporation of the pickling bath.
Les résultats obtenus exprimés en teneur de silice sont récapitulés dans le tableau ci-dessous :
Le procédé et le dispositif selon l'invention pour l'élimination substantielle des composés siliciques des bains de décapage, sont aisément transposables en milieu industriel et permettent d'obtenir de l'oxyde de fer dont la teneur en silice est inférieure à 100 ppm.The process and the device according to the invention for the substantial elimination of the silicic compounds from the pickling baths are easily transposable in an industrial environment and make it possible to obtain iron oxide whose silica content is less than 100 ppm.
Claims (9)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR9007519 | 1990-06-15 | ||
| FR9007519A FR2663344B1 (en) | 1990-06-15 | 1990-06-15 | PROCESS FOR SEPARATING SILICON COMPOUNDS FROM STRIPPING BATHS AND INSTALLATION FOR ITS IMPLEMENTATION. |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0463905A1 true EP0463905A1 (en) | 1992-01-02 |
| EP0463905B1 EP0463905B1 (en) | 1994-09-07 |
Family
ID=9397677
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP91401525A Expired - Lifetime EP0463905B1 (en) | 1990-06-15 | 1991-06-10 | Process for separating silicon compounds from pickling baths and apparatus therefor |
Country Status (7)
| Country | Link |
|---|---|
| US (1) | US5296001A (en) |
| EP (1) | EP0463905B1 (en) |
| JP (1) | JP3040201B2 (en) |
| AT (1) | ATE111164T1 (en) |
| DE (1) | DE69103825T2 (en) |
| ES (1) | ES2063463T3 (en) |
| FR (1) | FR2663344B1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0602758A1 (en) * | 1992-12-14 | 1994-06-22 | MANNESMANN Aktiengesellschaft | Process and apparatus for desludging acids |
| FR2916205A1 (en) * | 2007-05-16 | 2008-11-21 | Siemens Vai Metals Tech Sas | INSTALLATION AND PROCESS FOR TREATING SILICON STEEL BAND REMOVAL SOLUTIONS |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AT403697B (en) * | 1995-04-24 | 1998-04-27 | Chemikalien & Tech Service Ges | Process for removing silicic acid from aqueous, acid, preferably hydrochloric acid, solutions and preparation of low-silica metal oxide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1432661A (en) * | 1965-02-09 | 1966-03-25 | Loire Atel Forges | Improvements in the treatment of pickling baths for silicon steels |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4184955A (en) * | 1975-09-30 | 1980-01-22 | Arvanitakis Kostas S | Method and apparatus for clarifying liquids through settling |
| DE3019737C2 (en) * | 1980-05-23 | 1982-09-02 | Westfalia Separator Ag, 4740 Oelde | Centrifugal drum for clarifying and separating centrifugal liquids |
| JPS59111930A (en) * | 1982-12-16 | 1984-06-28 | Nippon Steel Corp | Process for preparation of iron oxide from hydrochloric acid pickling waste solution |
| JPS59169902A (en) * | 1983-03-14 | 1984-09-26 | Tadayoshi Karasawa | Improvement in procedures for waste acid purification |
| US4636317A (en) * | 1985-07-16 | 1987-01-13 | Fluid Recycling Services, Inc. | Recycling of metalworking fluids |
| JPS63144122A (en) * | 1986-12-03 | 1988-06-16 | Sumitomo Metal Ind Ltd | Method for removing silicon from hydrochloric acid-pickled waste liquid |
| JPS63144123A (en) * | 1986-12-08 | 1988-06-16 | Sumitomo Metal Ind Ltd | Method for removing silicon content in hydrochloric acid-pickled waste liquid |
| JPS63242932A (en) * | 1987-03-30 | 1988-10-07 | Sumitomo Metal Ind Ltd | Removal of silicon component from hydrochloric acid pickling waste liquid of steel material |
| JPH0742118B2 (en) * | 1987-12-10 | 1995-05-10 | 日本鋼管株式会社 | Method for purifying ferrous ion-containing acid solution |
-
1990
- 1990-06-15 FR FR9007519A patent/FR2663344B1/en not_active Expired - Lifetime
-
1991
- 1991-06-10 ES ES91401525T patent/ES2063463T3/en not_active Expired - Lifetime
- 1991-06-10 EP EP91401525A patent/EP0463905B1/en not_active Expired - Lifetime
- 1991-06-10 AT AT91401525T patent/ATE111164T1/en not_active IP Right Cessation
- 1991-06-10 DE DE69103825T patent/DE69103825T2/en not_active Expired - Fee Related
- 1991-06-14 JP JP3169267A patent/JP3040201B2/en not_active Expired - Fee Related
-
1993
- 1993-03-11 US US08/029,913 patent/US5296001A/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1432661A (en) * | 1965-02-09 | 1966-03-25 | Loire Atel Forges | Improvements in the treatment of pickling baths for silicon steels |
Non-Patent Citations (4)
| Title |
|---|
| PATENT ABSTRACTS OF JAPAN, vol. 12, no. 405 (C-539)[3252], 26 octobre 1988; & JP-A-63 144 123 (SUMITOMO METAL IND., LTD) 16-06-1988 * |
| PATENT ABSTRACTS OF JAPAN, vol. 13, no. 49 (C-565)[3397], 3 février 1989; & JP-A-63 242 932 (SUMITOMO METAL IND.) 07-10-1988 * |
| PATENT ABSTRACTS OF JAPAN, vol. 8, no. 225 (C-247)[1662], 16 octobre 1984; & JP-A-59 111 930 (SHIN NIPPON SEITETSU K.K.) 28-06-1984 * |
| PATENT ABSTRACTS OF JAPAN, vol. 9, no. 21 (C-263)[1744], 29 janvier 1985; & JP-A-59 169 902 (TADAYOSHI KARASAWA) 26-09-1984 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0602758A1 (en) * | 1992-12-14 | 1994-06-22 | MANNESMANN Aktiengesellschaft | Process and apparatus for desludging acids |
| FR2916205A1 (en) * | 2007-05-16 | 2008-11-21 | Siemens Vai Metals Tech Sas | INSTALLATION AND PROCESS FOR TREATING SILICON STEEL BAND REMOVAL SOLUTIONS |
| WO2008141716A1 (en) * | 2007-05-16 | 2008-11-27 | Siemens Vai Metals Technologies Sas | Equipment and method for processing pickling solutions for silicon steel strips |
Also Published As
| Publication number | Publication date |
|---|---|
| ATE111164T1 (en) | 1994-09-15 |
| JPH04231486A (en) | 1992-08-20 |
| US5296001A (en) | 1994-03-22 |
| EP0463905B1 (en) | 1994-09-07 |
| FR2663344A1 (en) | 1991-12-20 |
| FR2663344B1 (en) | 1992-10-09 |
| DE69103825T2 (en) | 1995-01-05 |
| ES2063463T3 (en) | 1995-01-01 |
| DE69103825D1 (en) | 1994-10-13 |
| JP3040201B2 (en) | 2000-05-15 |
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