EP1047638A1 - PROCEDE DE PREPARATION DE TiO 2? SELON LE PROCEDE AU SULFATE - Google Patents

PROCEDE DE PREPARATION DE TiO 2? SELON LE PROCEDE AU SULFATE

Info

Publication number
EP1047638A1
EP1047638A1 EP98966647A EP98966647A EP1047638A1 EP 1047638 A1 EP1047638 A1 EP 1047638A1 EP 98966647 A EP98966647 A EP 98966647A EP 98966647 A EP98966647 A EP 98966647A EP 1047638 A1 EP1047638 A1 EP 1047638A1
Authority
EP
European Patent Office
Prior art keywords
dryer
metatitanic acid
passed
calcination
moist
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.)
Withdrawn
Application number
EP98966647A
Other languages
German (de)
English (en)
Inventor
Matthias Kretschmer
Horst Ronkholz
Hans-Jürgen STOLL
Hartmut Wagner
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.)
Venator Germany GmbH
Original Assignee
Sachtleben Chemie GmbH
Metallgesellschaft AG
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 Sachtleben Chemie GmbH, Metallgesellschaft AG filed Critical Sachtleben Chemie GmbH
Publication of EP1047638A1 publication Critical patent/EP1047638A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
    • C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/08—Drying; Calcining ; After treatment of titanium oxide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity
    • C01P2006/82—Compositional purity water content

Definitions

  • the invention relates to a process for the production of Ti0 2 by the sulfate process.
  • the invention is therefore based on the object to provide a process for the production of Ti0 2 by the sulfate process, in which the energy consumption is relatively low and in which S0 3 -, S0 2 - and dust-containing exhaust gases occur in the smallest possible amount.
  • the thermal action on the titanium dioxide in the calcination furnace is to be evened out by narrowing the grain spectrum of the metatitanic acid agglomerates.
  • the object on which the invention is based is achieved in that the moist metatitanic acid filter cake is passed through a dryer for calcination before entering the oven and is predried there to a residual moisture content of 0.01 to 25% at 100 to 190.degree.
  • the moist metatitanic acid cake shows usually a relative humidity of 40 to 60%.
  • a rotary kiln can be used as the calcining furnace.
  • the residual moisture is to be understood as the mass of water that corresponds to the mass of the moist
  • Hot filter press can also advantageously be used as the dryer, in which predrying to a residual moisture content of 5 to 25% can be carried out in a relatively simple manner.
  • Hot filter presses are frame or chamber filter presses, the hollow filter plates of which can be charged from the inside with hot media, such as steam, in order to dry the filter cake in the filter.
  • the energy consumption can be reduced in a particularly advantageous manner by the process according to the invention, at the same time improving the pigment properties such as spreading power, brightness and gloss.
  • the energy to be supplied to the calcination furnace in the sulfate process according to the prior art is required to a very large extent for dewatering the metatitanic acid. It also serves to split off the sulfate group and residual sulfuric acid adhering to the metatitanic acid, with SO 3 and SO 2 being formed. To a lesser extent, the energy to be supplied is used to heat and convert the metatitanic acid into Ti0 2 . Since S0 2 and S0 3 are formed in the calcination furnace, the dew point of the furnace exhaust gas is increased compared to an exhaust gas containing only water vapor.
  • flue gas temperatures of the calcination furnace are known Sulphate process / set above 300 ° C, which would actually not be necessary to drain the metatitanic acid.
  • the calcination furnace is therefore supplied with more energy only to avoid corrosion damage than would actually be necessary to dewater the metatitanic acid, to split off the sulfate group and residual sulfuric acid adhering to the metatitanic acid and to convert the metatitanic acid into Ti0 2 .
  • the amount of exhaust gas is reduced by the lack of water vapor in the pre-dried material.
  • the downstream exhaust gas cleaning systems for removing S0 3 S0 2 and dust can advantageously be designed to be smaller due to the smaller amount of exhaust gases.
  • the pigment quality is improved by the process according to the invention, since it is advantageous for the calcination Can set primary particle size of about 0.3 microns, the grain spectrum is relatively narrow.
  • a preferred embodiment of the invention is that a temperature of 110 to 160 ° C is set in the dryer. If a temperature of 110 to 160 ° C is set in the dryer, it is ensured that the cleavage of the sulfate group and residual sulfuric acid adhering to the metatitanic acid in the dryer is completely avoided, with the result that the exhaust gases removed from the dryer are free of SO 3 and S0 2 and therefore do not have to be routed through additional exhaust gas purification systems.
  • the moist metatitanic acid filter cake is passed through a grinding dryer arranged as a dryer. Due to the adjustment of the temperature and residence time of the material, the moisture content and the grain spectrum of the resulting metatitanic acid agglomerates can be controlled in a particularly advantageous manner in the grinding dryer.
  • the moist metatitanic acid filter cake is generated in a drum filter before entering the dryer and there is pre-dewatered to an absolute humidity of 55 to 65% and then passed through a spray dryer arranged as a dryer.
  • the moist metatitanic acid filter cake removed from the drum filter has properties similar to those of a liquid, so that the drying can then advantageously be carried out in a spray dryer.
  • it is provided that the moist metatitanic acid filter cake is produced before entering the dryer in a membrane chamber filter press and there is pre-dewatered to an absolute humidity of 40 to 55% and then passed through a grinding dryer arranged as a dryer. The moisture removed from the membrane filter chamber press
  • Metatitanic acid filter cake is in lumpy form, so that drying can advantageously take place in the downstream grinding dryer.
  • the pre-dewatering in the membrane chamber filter press advantageously reduces the energy consumption in the subsequent drying step.
  • the pre-dewatered metatitanic acid filter cake is passed through a plate dryer arranged as a dryer and pre-dried to a residual moisture content of 5 to 25%.
  • the pre-dewatered metatitanic acid filter cake is in lumpy form, so that drying can be carried out particularly advantageously in a plate dryer.
  • the exhaust gases discharged from the furnace for calcination are passed as hot gases through the dryer.
  • the exhaust gases discharged from the furnace for calcination generally have a temperature of approximately 450 ° C. and are therefore advantageously suitable as hot gases for the dryer.
  • the exhaust gases removed from the dryer in this procedure must, however, then be freed of SO 3 and SO 2 .
  • Na ⁇ h a further preferred embodiment of the invention, it is provided that the exhaust air of the dryer and / or the discharged from the furnace for calcination exhaust gases are used for preheating the hot gases for the dryer. Heat exchangers are arranged.
  • the exhaust gases discharged from the dryer are also advantageously suitable for preheating the hot gases, since they generally have a temperature of approximately 120 ° C.
  • the predried metatitanic acid filter cake is comminuted to an average grain size of 0.1 to 4 mm immediately before entering the oven for calcination. This has an advantageous effect on the calcination process, since an advantageous, uniform heating is achieved in the kiln for the calcination.
  • the figure shows a simplified schematic
  • Fig. A simplified process flow diagram of the process for the production of Ti0 2 by the sulfate process is shown.
  • the wet metatitanic acid filter cake (1) that is obtained in the filter which can be designed, for example, as a membrane chamber filter press, is passed into the dryer (2), which is then advantageously designed as a grinding dryer.
  • the moist metatitanic acid filter cake (1) introduced into the dryer (2) generally has a relative one Moisture from 40 to 60%.
  • Hot gases (3) are introduced into the dryer (2) and the exhaust gases are discharged via line (4).
  • the hot gases (3) introduced into the dryer (2) can advantageously have been preheated by process gases.
  • the exhaust gases leave the dryer (2) at a temperature of approx. 120 ° C. In the dryer (2) the damp
  • the pre-dried metatitanic acid filter cake is fed via line (5) to the furnace (6) for calcination, optionally after pre-comminution to an average grain size of 0.1 to 4 mm.
  • the calcining furnace (6) is usually a rotary kiln. Fuels (7) are fed to the calcining furnace (6), gas or oil being used. It is only in the furnace (6) for calcination that the sulfate group and residual sulfuric acid adhering to the metatitanic acid are split off, SO and SO 3 being formed. Furthermore, the conversion of the metatitanic acid into Ti0 2 takes place via the line (8) from the furnace
  • the S0 2 - and S0 3 -containing exhaust gases are fed via line (9) to a quench cooler (10) which is supplied with water via line (11).
  • the cooled exhaust gases are then fed via line (12) to an electrostatic precipitator (13), in which they are freed from SO 3 .
  • the exhaust gases freed from SO reach the scrubber (15) via line (14), in which SO is separated.
  • the exhaust gases freed from SO and SO pass through line (16) and the chimney

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

L'invention concerne un procédé selon lequel il est prévu qu'avant l'entrée dans le four (6) destiné à la calcination, le gâteau de filtration d'acide métatitanique (1) soit acheminé à travers un séchoir (2) et qu'il y soit préséché à une température comprise entre 100 et 190 °C jusqu'à ce que son humidité résiduelle soit de l'ordre de 0,01 à 25 %.
EP98966647A 1998-01-13 1998-12-19 PROCEDE DE PREPARATION DE TiO 2? SELON LE PROCEDE AU SULFATE Withdrawn EP1047638A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19800881 1998-01-13
DE1998100881 DE19800881A1 (de) 1998-01-13 1998-01-13 Verfahren zur Herstellung von TiO¶2¶ nach dem Sulfatverfahren
PCT/EP1998/008341 WO1999036362A1 (fr) 1998-01-13 1998-12-19 PROCEDE DE PREPARATION DE TiO2 SELON LE PROCEDE AU SULFATE

Publications (1)

Publication Number Publication Date
EP1047638A1 true EP1047638A1 (fr) 2000-11-02

Family

ID=7854422

Family Applications (1)

Application Number Title Priority Date Filing Date
EP98966647A Withdrawn EP1047638A1 (fr) 1998-01-13 1998-12-19 PROCEDE DE PREPARATION DE TiO 2? SELON LE PROCEDE AU SULFATE

Country Status (5)

Country Link
EP (1) EP1047638A1 (fr)
DE (1) DE19800881A1 (fr)
PL (1) PL341766A1 (fr)
SI (1) SI20322A (fr)
WO (1) WO1999036362A1 (fr)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100448783C (zh) * 2004-12-09 2009-01-07 江苏大学 一种制备锐钛矿型纳米TiO2的方法
CN100335416C (zh) * 2005-04-18 2007-09-05 江苏大学 以羧酸为修饰剂低温制备金红石型纳米TiO2的方法
WO2012017315A1 (fr) * 2010-08-04 2012-02-09 Flsmidth A/S Procédé de séchage d'un gâteau de boues au moyen des gaz d'échappement d'un four de calcination
US11440513B2 (en) 2020-06-04 2022-09-13 Bendix Commercial Vehicle Systems, Llc Parking brake for an electric vehicle with multi-speed gearbox
CN113428895B (zh) * 2021-08-06 2022-10-28 龙佰四川钛业有限公司 一种硫酸法偏钛酸的煅烧方法
CN113582228B (zh) * 2021-08-13 2022-06-03 广东惠云钛业股份有限公司 一种高白度钛白粉的制备方法及应用

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3689219A (en) * 1971-05-24 1972-09-05 Vanderbilt Co R T Process of precipitating h2tio3
DE3630220A1 (de) * 1986-09-05 1988-03-10 Bayer Ag Verfahren zur herstellung von titandioxidpigmenten
DE3840195A1 (de) * 1988-11-29 1990-05-31 Bayer Ag Titandioxid, verfahren zu seiner herstellung und dessen verwendung
DE3921262C1 (fr) * 1989-06-29 1990-07-05 Bayer Ag, 5090 Leverkusen, De
US5744108A (en) * 1996-01-15 1998-04-28 Bayer Ag Process for the thermal treatment of titanium dioxide in a circulating fluidized bed and the use thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9936362A1 *

Also Published As

Publication number Publication date
SI20322A (sl) 2001-02-28
PL341766A1 (en) 2001-05-07
DE19800881A1 (de) 1999-07-15
WO1999036362A1 (fr) 1999-07-22

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