DE2004878C3 - Process for enriching the titanium oxide content in titanium ores - Google Patents

Description

Hydrogen acid in the steam tube with the use of the leach mixture in the digester in such a way as to add the from the treatment of the lye. improve that emer under avoidance ^ heat recovered hot lOprozentigen HCl up also vessel from outside the content ausschheßhch by _heating means is heated, the acid concentration in the

Inside the digester not changed significantly and

does not affect the cost-effectiveness of the process

a5 is pregnant, but on the contrary increases.

This problem was solved by the invention

The invention relates to the processing of general processes for the enrichment of titanium dioxide or other iron-containing titanium ores, such as the content of iron-containing titanium ores or titanium and Ilmenite-magnetite, hmenite-hematite, or from slag containing titanium iron oxide by leaching the contained Magnetite or Hämattt or titanium or iron 3 »reduced starting material in the digester at up to oxide-containing slags by extracting iron about 143 ° C under a pressure of up to 3.5 atu and other acid-soluble components with chlorine with liquid, aqueous-azeotropic 20% hydrochloric acid, the latter consisting of the chemical acid, separating the undissolved titanium extraction waste eyes obtained recovered dioxides, recovery of which is contained in the waste liquor. In the work-up, Iimenit is obtained as 35 NEN proportions of hydrogen chloride by transferring the so-called "synthetic rutile" an enriched iron chloride dissolved in it in iron oxide and jerks Iimenit with a high titanium dioxide content and low levels of the released hydrogen chloride in the Iron content, which has particularly good properties- leaching vessel, which is characterized in that and in particular as a raw material for her- man the leach mixture in the digester exclusively Position of titanium tetrachloride, of titanium dioxide pigments- 4 ° by introducing 20 weight percent aqueous th and other titanium compounds through the "chloro-hydrochloric acid in vapor form with Mitverrierungs" - (or "Chloride") method is suitable. Turning of the from the treatment of the waste liquors

Natural rutile is currently the most important raw material - recovered hot 20 percent HCI heats, material for the production of titanium dioxide pigment with When carrying out the method according to the invention

With the help of the above-mentioned chlorination process, the titanium-containing ore or the slag is added, but due to the limited P. B. due to the ability to heat the "synthetic rutile" more and more importantly with coke to around 815 to 1000 ⁰ C or more, as a substitute for natural rutile, if only because the main proportion of ferrous iron in ferrous iron is more versatile than natural, The transfer and at the same time the crystal lattice of the ore he also has important properties, in particular to break open so that the acid is better than the porosity of the iron, so that it can be attacked in the aforementioned.

Reaction with chlorine gas creates a larger contact area. The pre-reduced raw material is then put into a

having. vessel with an acid-proof lining (Dig-

Many attempts have therefore already been made to abandon the ester). In the vessel that was used during the dige-ilmenite or other iron-containing titanium ores to be processed is kept in slow rotation tt:;, j ^ loch only led a few to success. The only hot, 20 weight percent hydrochloric acid einbis Some time ago technically applied processes were carried out.

Ut the preparation of Iimenit by leaching with the extraction (leaching) that

3l, 5% hydrochloric acid (HCl of 20 ° B6). Usual two-stage, countercurrent VeriNoch A few years ago, 60 drives were used in this way. However, the warm-up takes place in the commercial quantities of processed Iimenit present case exclusively with 20% HCl · · toonne & j, however, had to produce from economic steam, which is prepared in an HCl evaporator, borrowed reasons and because waste problems arose while with known methods for heating and are given. In particular, the high hydrochloric acid ratio to maintain the digestion the need and the elimination of the large amounts of at- 65 temperatures and pressures in the digester immediately Falling ferric chloride solution made the procedure water vapor was initiated. According to the invention ünwifischaftlbh and unsuitable for practice. a dilution of the acid with steam

The aim was therefore to avoid the decomposition of the condensate alone and in the reaction mixture

3 '4

during the entire digestion period the acid concentration is different for the various

Maintain the most complete acid concentration. guided pressures

The literature shows that when used, the waste liquor from the first leaching stage contains of steam for heating the Me age to Kon- as in the known processes, which all dem densat depends on many factors, some of which, 5 ore-extracted iron in the form of chloride in addition to something like loss of heat, etc., not readily conspicuous acid. It turns into hydrochloric acid are trollable. As a result, the reuse recovered varies, with as ancillary propose Process the acid concentration of Ctsrge duct iron oxide is obtained, which is sent to Suhlwerke Batch, which of course means that the quality of the sample can be given. The acid is obtained duktes ebenCaäs is subject to strong fluctuations in the usual way, e.g. B. using the "Aman" method Is on the other hand used exclusively 20% or in another known recovery vapor form HCl for heating up, so the problem is device.

of the fluctuation in the acid concentration from batch to batch.As is well known, a hydrochloric acid of 20% by weight per batch is overcome, and one centimeter of titanium is obtained, the highest concentration that can be obtained with the above-mentioned oxide of more uniform nature 15 or other known recovery-For an ilmenite with 55 to 60% TiO ₈ is z. B. procedure can receive. The use of this hot 20% HCl per 1 part ilmenite, which is indirectly obtained during the recovery and the total consumption of acid is about 2.6 parts by weight a titanium-containing the inventive feature of the use of slag from the iron content and the acid-soluble components present in addition to the 20-20% hydrochloric acid in vapor form to the titanium. In order to heat up the digester, the expensive and time-consuming extraction of iron and other acid-releasing concentration of the 20% HCl, which ensures borne substances in the ore, is saved, if the azeotropic, constant-boiling mixture is used, moderately for a stoichiometric acid over- to a higher concentration, which would be indispensable, shot from 15 to 20 percent by weight. In the first leaching stage, if steam is used for heating, the prereduced raw material is ex-d. In addition, this measure enables traction with a mixture that consists of the process with a higher degree of efficiency durchzulauge from the second leaching stage a preceding-lead than the known processes in which with the batch plus recovered HCl (Korzen- stronger HCl leached and steamed up 20 percent by weight) in an amount that heats the 30. In addition, the half of the total acid requirement accruing according to the invention (see above) is ent- titanium dioxide of particularly uniform composition. Used for leaching in the second stage.

the remaining amount, d. H. the other half of the process according to the invention is now through a

total acid requirement, in the form of 20% HCl. As the example explains in more detail,

20% HCl vapor used as heating medium 35 η · · 1

becomes some chlorine example during the leaching

hydrofluoric acid condensed; the amount depends on by heating with coke for 40 minutes

the construction or the heat loss of the Dige - about 90O ⁰ C was a "Quilon" won in India -

riergefäßes, pre-reduced by the leaching time and by the primary ilmenite of the following composition:

initial temperature of the batches and the pre 40 -j-jq 59 55 y

direction. p _e q 22737

If you want to achieve a particularly good extraction, then p_Q ³ 10777

It is expedient to use both Al 0 leaching stages 1 * 447

under a pressure of about 1.4 to 3.5 atmospheres and at gjQ ^s 1 * 41 y

at a temperature between about 108 and 145 ° C. 45 _Kes \ other 'oxides' etc!
Under these conditions each leaching stage lasts

about 5 hours. The exact time required depends on even 1 part by weight of the pre-reduced ilmenite was used

understandable from the nature and characteristics of the then leached in two stages, including a total of

Raw material. In the case of ilmenite, 2.6 parts by weight (15% excess) are heated ^{to 100 ° C., as found}

was, in the acid up to 94% of the iron content fresh 20% HCl was used; every stage

solves. The residue contains about 98% of the original - took 5 hours and it was made with 20%

borrowed TiO ₈ present. HCl steam of 100 ⁰ C directly heated.

In the process according to the invention, after separating and drying, the

Stages a constant boiling azeotropic mixture of ridden ilmenite the following composition:

HCl and water present, the composition of which is 55 jjq 92,127

and boiling point from the prevailing pressure - Fe O 210 7

hangs. For example, the constant boiling p_k * n \ c ° /

Acid mixture at 760 mm Hg 20.22% HCl (boiling ^{/ o}

⁰ point 108.58 C), at 1000 mm Hg it contains 19.73% The weight ratio of treated ilmenite

HCl and boiling at 116.18 ° C, at 1200 mm Hg contains 60 to raw material was 63: 100. The iron turned to

it 19.42% HCl and boils at 122.38 ° C. The re-extracted 93.7%, and the yield based on

recovered HCl is on average about 20%, and this TiO ₈ , was 97.5%.

1 sheet of drawings

Claims (1)

falling iron morids and the reuse of rn »; <H> ci> t7ten hydrochloric acid, and the more recent literature Godfather ^ spruca: KSÄSge to refer to this Sleep * n * The iron chloride dissolved in it is covered by the introduction of steam . The digester is characterized by the fact that the concentration of HCl is carried out