CN109809469A

CN109809469A - The method of low melting point complex in side reaction is removed in a kind of production of titanium chloride

Info

Publication number: CN109809469A
Application number: CN201711160796.7A
Authority: CN
Inventors: 田长对
Original assignee: Individual
Current assignee: Individual
Priority date: 2017-11-20
Filing date: 2017-11-20
Publication date: 2019-05-28

Abstract

The method of low melting point complex in side reaction is removed in a kind of production of titanium chloride, when fused salt chlorimation method produces titanium chloride, contain the titanium chloride gas of chloride impurity after dust-precipitator gathers dust in the high temperature that Molten salt chlorination furnace generates, it is eluted into eluting column with titanium chloride liquid, in elution column overhead, one water spray spray head is set, the water spray spray head is set to carry out shower water by being passed through chlorine, into the NaAlCl4 carried secretly in the water and titanium chloride gas in eluting column, reaction is hydrolyzed in NaFeCl4 low melting point complex and AlCl3, generate aluminium oxide and iron oxide, as titanium chloride enters in the elution slot of eluting column, it is mixed into mud, then the mud eluted in slot dust-precipitator is back to gather dust.Advantage is: can remove NaAlCl4, NaFeCl4 low melting point complex in side reaction, guarantees fused salt chlorimation reactor assembly long-time steady operation.

Description

The method of low melting point complex in side reaction is removed in a kind of production of titanium chloride

Technical field

The present invention relates to the methods that low melting point complex in side reaction is removed in a kind of production of titanium chloride.

Background technique

Currently, large-scale fused salt chlorimation production technology has been mature technology at home, the alumina component in rich-titanium material is being matched Chlorination can occur in carbon chlorination process and generate AlCl₃, chlorination rate is generally up to 50% or more.AlCl₃It is layer structure in solid-state, Al is translated into when close to its melting temperature₂Cl₆Molecular structure, and gas phase is volatized into dimer vapors molecule；Work as temperature After degree further increases, dimer molecule is decomposed into AlCl again₃Molecule.In fused salt chlorimation system, FeCl₃Behavior and AlCl₃Class Seemingly.In fused salt chlorimation reactor, product AlCl₃、FeCl₃It may be with the NaCl or KCl formation saturated vapor in molten salt system Press relatively low chloride complexes NaAlCl₄、NaFeCl₄, influence the stable fortune of long period in fused salt chlorimation production process Row, especially NaAlCl₄、NaFeCl₄Fusing point is low, is not easy to remove, be mixed in the titanium chloride of generation, as titanium chloride moves back；This Under the dust-precipitator and eluting column temperature gradient of post-processing, the complex of this kind of low melting point successively condenses out sample, gradually bonds In the wall of dust-precipitator and eluting column, it can make to bond more complex on system wall quickly, can only stop in process of production Heat preservation is produced, carries out physics operation to the NaAlCl being bonded in system₄、NaFeCl₄Low melting point complex is cleared up, and system is influenced Long-term operation.

Take into account dust collection effect and chlorination titanium recovery rate, afterbody dust-precipitator flue gas exit temperature need to control 190 DEG C~ 200℃.The temperature is higher than NaAlCl₄、NaFeCl₄And AlCl₃Boiling point, this makes NaAlCl₄、NaFeCl₄And AlCl₃Largely into Enter eluting column and fails as FeCl₃It equally removes in dust-precipitator, is discharged in the form of dust-slag collection.Due to scrubbed in eluting column The thick titanium chloride underflow slurry generated, which directly returns, gathers dust or chlorination system, will gasify again, to gather dust-elute in chlorination- Continuous circulative accumulation in system, not only increases system burden, also easily causes system knot wall, dust-slag collection local liquefaction, heat exchange The problems such as device fouling, influences the stability of chlorination operation.In addition, NaAlCl₄、NaFeCl₄With a small amount of AlCl₃Can also To subsequent TiCl₄Purification and titanium sponge production cause adverse effect, and as a kind of very strong lewis acid of acidity, set to steel It is standby that there is very strong corrosivity.Bigger difficulty is caused to the period of steady production chlorination titanium products.

Summary of the invention

The technical problem to be solved in the present invention is to provide remove low melting point complex in side reaction in a kind of production of titanium chloride Method.

The technical solution of the invention is as follows:

The method that low melting point complex in side reaction is removed in a kind of production of titanium chloride, comprises the concrete steps that:

When fused salt chlorimation method produces titanium chloride, contain the titanium chloride gas of chloride impurity in the high temperature that Molten salt chlorination furnace generates Body is eluted after dust-precipitator gathers dust, into eluting column with titanium chloride liquid, and titanium chloride gas flow is 1000m³/ h~ 1100m³/ h, temperature are 220 DEG C, and a water spray spray head is arranged in elution column overhead, makes the water spray by being passed through chlorine Spray head carries out shower water, and the pressure of chlorine is 0.45Mpa, flow 12m³/ h, spray water flow are 20kg/h~24kg/h, leaching It washes temperature in tower to control at 180 DEG C~200 DEG C, into the NaAlCl carried secretly in the water and titanium chloride gas in eluting column₄、 NaFeCl₃Low melting point complex and AlCl₃Reaction is hydrolyzed, aluminium oxide and iron oxide are generated, as titanium tetrachloride enters leaching It washes in the elution slot of tower, is mixed into mud, the mud eluted in slot is then back to dust-precipitator and carries out dust-precipitator, in mud Aluminium oxide and iron oxide gather dust in dust-precipitator at solid state.

Beneficial effects of the present invention:

At moderate temperatures, NaAlCl₄、NaFeCl₄Low melting point complex and AlCl₃Prior to TiCl₄It hydrolyzes, The NaAlCl being introduced into water selective hydrolyzation system in right amount₄、NaFeCl₄And AlCl₃, it is allowed to be changed into solid oxide, with mud Slurry form returns to the tower that gathers dust and gathers dust, so as to avoid NaAlCl₄、NaFeCl₄Wall built-up of the equal low-boiling point materials in eluting column is existing As guaranteeing fused salt chlorimation reactor assembly long-time steady operation.

Specific embodiment

Embodiment

When fused salt chlorimation method produces titanium chloride, contain chloride impurity (predominantly chlorine in the high temperature that Molten salt chlorination furnace generates Change aluminium and iron chloride) titanium chloride gas after dust-precipitator gathers dust, eluted into eluting column with titanium chloride liquid, four chlorinations Titanium gas flow is 1000m³/ h, temperature are 220 DEG C, increase a water spray spray head in elution column overhead, by being passed through nitrogen The water spray spray head is set to carry out shower water, the pressure of chlorine is 0.45Mpa, flow 12m³/ h, spray water flow 20kg/ H, temperature control is at 180 DEG C in eluting column, into the NaAlCl carried secretly in the water and titanium chloride gas in eluting column₄、NaFeCl₄ Low melting point complex and AlCl₃Reaction is hydrolyzed, aluminium oxide and iron oxide are generated, as titanium chloride enters the leaching of eluting column In washing trough, be mixed into mud, the mud eluted in slot be then back to dust-precipitator and carries out dust-precipitator, aluminium oxide in mud and Iron oxide gathers dust in dust-precipitator at solid state, is discharged as dust-slag collection, and Al content is 20% in the dust-slag collection in the tower that gathers dust, It can guarantee system long-period stable operation without wall built-up phenomenon substantially in eluting column.

Claims

1. a kind of method for removing low melting point complex in side reaction in titanium chloride production, it is characterized in that: fused salt chlorimation method produces When titanium chloride, in the titanium chloride gas that the high temperature that Molten salt chlorination furnace generates contains chloride impurity after dust-precipitator gathers dust, enter Eluting column is eluted with titanium chloride liquid, and titanium chloride gas flow is 1000m3/h~1100m3/h, temperature is 220 DEG C, It elutes column overhead and one water spray spray head is set, so that the water spray spray head is carried out shower water, the pressure of chlorine by being passed through chlorine Power is 0.45Mpa, flow 12m3/h, and spray water flow is 20kg/h~24kg/h, in eluting column temperature control 180 DEG C~ 200 DEG C, into NaAlCl4, NaFeCl4 low melting point complex for carrying secretly in the water and titanium chloride gas in eluting column and Reaction is hydrolyzed in AlCl3, generates aluminium oxide and iron oxide as titanium chloride enters in the elution slot of eluting column and is mixed into mud In, the mud eluted in slot is then back to dust-precipitator and carries out dust-precipitator.