EP0463905A1 - Verfahren zur Entfernung von Siliziumverbindungen aus Beizbädern und Einrichtung dafür - Google Patents

Verfahren zur Entfernung von Siliziumverbindungen aus Beizbädern und Einrichtung dafür Download PDF

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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
Authority
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.)
Granted
Application number
EP91401525A
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English (en)
French (fr)
Other versions
EP0463905B1 (de
Inventor
Lothaire Walter Scherer
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sollac SA
Original Assignee
Sollac SA
Lorraine de Laminage Continu SA SOLLAC
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Sollac SA, Lorraine de Laminage Continu SA SOLLAC filed Critical Sollac SA
Publication of EP0463905A1 publication Critical patent/EP0463905A1/de
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Anticipated expiration legal-status Critical
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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)
EP91401525A 1990-06-15 1991-06-10 Verfahren zur Entfernung von Siliziumverbindungen aus Beizbädern und Einrichtung dafür Expired - Lifetime EP0463905B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9007519 1990-06-15
FR9007519A FR2663344B1 (fr) 1990-06-15 1990-06-15 Procede de separation de composes siliciques des bains de decapage et installation pour sa mise en óoeuvre.

Publications (2)

Publication Number Publication Date
EP0463905A1 true EP0463905A1 (de) 1992-01-02
EP0463905B1 EP0463905B1 (de) 1994-09-07

Family

ID=9397677

Family Applications (1)

Application Number Title Priority Date Filing Date
EP91401525A Expired - Lifetime EP0463905B1 (de) 1990-06-15 1991-06-10 Verfahren zur Entfernung von Siliziumverbindungen aus Beizbädern und Einrichtung dafür

Country Status (7)

Country Link
US (1) US5296001A (de)
EP (1) EP0463905B1 (de)
JP (1) JP3040201B2 (de)
AT (1) ATE111164T1 (de)
DE (1) DE69103825T2 (de)
ES (1) ES2063463T3 (de)
FR (1) FR2663344B1 (de)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0602758A1 (de) * 1992-12-14 1994-06-22 MANNESMANN Aktiengesellschaft Verfahren und Vorrichtung zur Säureentschlammung
FR2916205A1 (fr) * 2007-05-16 2008-11-21 Siemens Vai Metals Tech Sas Installation et procede pour le traitement de solutions de decapage de bandes d'acier au silicium

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AT403697B (de) * 1995-04-24 1998-04-27 Chemikalien & Tech Service Ges Verfahren zur entkieselung von wässrigen, sauren, vorzugsweise salzsauren lösungen sowie herstellung von kieselsäurearmem metalloxid

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1432661A (fr) * 1965-02-09 1966-03-25 Loire Atel Forges Perfectionnements apportés au traitement des bains de décapage des aciers au silicium

Family Cites Families (9)

* Cited by examiner, † Cited by third party
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 (de) * 1980-05-23 1982-09-02 Westfalia Separator Ag, 4740 Oelde Schleudertrommel zum Klären und Trennen von Schleuderflüssigkeiten
JPS59111930A (ja) * 1982-12-16 1984-06-28 Nippon Steel Corp 塩酸酸洗廃液から酸化鉄を製造する方法
JPS59169902A (ja) * 1983-03-14 1984-09-26 Tadayoshi Karasawa 廃酸精製処理工程の改良
US4636317A (en) * 1985-07-16 1987-01-13 Fluid Recycling Services, Inc. Recycling of metalworking fluids
JPS63144122A (ja) * 1986-12-03 1988-06-16 Sumitomo Metal Ind Ltd 塩酸酸洗廃液からけい素を除去する方法
JPS63144123A (ja) * 1986-12-08 1988-06-16 Sumitomo Metal Ind Ltd 鋼材の塩酸酸洗廃液中のけい素分の除去方法
JPS63242932A (ja) * 1987-03-30 1988-10-07 Sumitomo Metal Ind Ltd 鋼材の塩酸酸洗廃液中のけい素分の除去方法
JPH0742118B2 (ja) * 1987-12-10 1995-05-10 日本鋼管株式会社 第一鉄イオン含有酸溶液の精製方法

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1432661A (fr) * 1965-02-09 1966-03-25 Loire Atel Forges Perfectionnements apportés au traitement des bains de décapage des aciers au silicium

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0602758A1 (de) * 1992-12-14 1994-06-22 MANNESMANN Aktiengesellschaft Verfahren und Vorrichtung zur Säureentschlammung
FR2916205A1 (fr) * 2007-05-16 2008-11-21 Siemens Vai Metals Tech Sas Installation et procede pour le traitement de solutions de decapage de bandes d'acier au silicium
WO2008141716A1 (fr) * 2007-05-16 2008-11-27 Siemens Vai Metals Technologies Sas Installation et procede pour le traitement de solutions de decapage de bandes d'acier au silicium

Also Published As

Publication number Publication date
ATE111164T1 (de) 1994-09-15
JPH04231486A (ja) 1992-08-20
US5296001A (en) 1994-03-22
EP0463905B1 (de) 1994-09-07
FR2663344A1 (fr) 1991-12-20
FR2663344B1 (fr) 1992-10-09
DE69103825T2 (de) 1995-01-05
ES2063463T3 (es) 1995-01-01
DE69103825D1 (de) 1994-10-13
JP3040201B2 (ja) 2000-05-15

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