CN103626224B - Fused salt chlorination furnace for producing titanium tetrachloride - Google Patents
Fused salt chlorination furnace for producing titanium tetrachloride Download PDFInfo
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- CN103626224B CN103626224B CN201310604232.3A CN201310604232A CN103626224B CN 103626224 B CN103626224 B CN 103626224B CN 201310604232 A CN201310604232 A CN 201310604232A CN 103626224 B CN103626224 B CN 103626224B
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Abstract
The invention discloses a fused salt chlorination furnace for producing titanium tetrachloride. A return slurry ore pipe, a feed pipe, an explosion-proof port and a product mixed steam discharge port are formed in the top of the fused salt chlorination furnace; a side salt discharge pipe, a plurality of chlorine pipes and a plurality of heating electrodes are arranged at a side part of the fused salt chlorination furnace; a bottom salt discharge pipe is arranged at the bottom of the fused salt chlorination furnace; the furnace wall of the fused salt chlorination furnace comprises three layers, wherein the outer layer is a metal furnace shell, the middle layer is a buffer packed layer and the inner layer is a fire brick layer; a circle of nozzle plugs are arranged on the outer walls of the chlorine pipes; a circle of electrode lug blocks are arranged on the outer surfaces of the heating electrodes. The fused salt chlorination furnace disclosed by the invention is simple in structure, can prevent gas leakage, and can regularly discharge waste salts and improve the chlorination environment to facilitate production of TiCl4.
Description
Technical field
The invention belongs to field of chemical metallurgical technology, more particularly, relate to the Molten salt chlorination furnace utilizing fused salt chlorimation method to produce titanium tetrachloride.
Background technology
The TiCl of present main flow
4production method is that fluidizing chlorination method produces TiCl
4but fluidizing chlorination method produces TiCl
4high to the grade requirement of titanium slag, also relatively stricter to the requirement of the granularity of titanium slag, require that the impurity component in titanium slag is relatively low, particularly the content sum of CaO and MgO requires to be less than 2%.Further, fluidizing chlorination method produces TiCl
4temperature requirement higher, need reach more than 900 DEG C, the waste gas of production is based on CO, and CO is hazardous gas, has the danger of blasting.
And fused salt chlorimation method produces TiCl
4these problems would not be had, and for mining heritages CaO, feature that content of MgO is high, select fused salt chlorimation method to produce TiCl
4more applicable.In Molten salt chlorination furnace, fused salt is mainly with NaCl, CaCl
2and MgCl
2be main Deng muriate, be present in liquid form in Molten salt chlorination furnace after the temperature of fused salt reaches 750 ~ 780 DEG C.The waste gas that fused salt chlorimation method is produced is with CO
2be main, directly enter in air to produce environment and pollute and impact.
The feature of Molten salt chlorination furnace comprises: (1) is not too high to the grade requirement of titanium slag, can process CaO, titanium slag that content of MgO is high; (2) lower to the granularity requirements of titanium slag, and particle size distribution is wider; (3) composition of the CTT produced is relatively good, and it is lower that thick CTT cleans foreign matter content; (4) waste gas is with CO
2be main, the danger also not having blast free from environmental pollution, CO
2need not process and can directly enter in air.
Summary of the invention
In order to solve the deficiencies in the prior art, the object of the present invention is to provide a kind of Molten salt chlorination furnace for the production of titanium tetrachloride, producing TiCl to solve fused salt chlorimation method
4produced problem in process.
To achieve these goals, the invention provides a kind of Molten salt chlorination furnace of producing titanium tetrachloride, the top of described Molten salt chlorination furnace is arranged returns slurry pipe, filling tube, venting and resultant mixing steam discharge port, the sidepiece of described Molten salt chlorination furnace arranges side salt discharging pipe, many Chlorination tubes and multiple heating electrode, the bottom of described Molten salt chlorination furnace arranges end salt discharging pipe, and the furnace wall of described Molten salt chlorination furnace comprises three layers, wherein, skin is metal furnace shell, middle layer is buffer fillings layer, internal layer is fire brick layer, the outer wall of described Chlorination tube is arranged a circle nozzle plug, the outside surface of described heating electrode arranges a circle electrode ear block.
According to an embodiment of the Molten salt chlorination furnace of production titanium tetrachloride of the present invention, described Molten salt chlorination furnace also comprises the thermopair and pressure warning unit that are arranged at top, and is arranged at sidepiece to insert the fused salt thermopair of fused salt in stove.
According to an embodiment of the Molten salt chlorination furnace of production titanium tetrachloride of the present invention, described fused salt thermopair comprises the pottery of outer field corundum and internal layer.
According to an embodiment of the Molten salt chlorination furnace of production titanium tetrachloride of the present invention, one end of described heating electrode connects power supply and the other end to insert in stove in fused salt.
According to an embodiment of the Molten salt chlorination furnace of production titanium tetrachloride of the present invention, described Molten salt chlorination furnace comprises three heating electrodes, and described three heating electrodes are mutually hexagonal angle and arrange.
According to an embodiment of the Molten salt chlorination furnace of production titanium tetrachloride of the present invention, described Molten salt chlorination furnace comprises four Chlorination tubes, and described Chlorination tube inserts and leads to the bottom of fused salt in stove.
According to an embodiment of the Molten salt chlorination furnace of production titanium tetrachloride of the present invention, described side salt discharging pipe and end salt discharging pipe also comprise salt discharge shutoff plug, and side salt discharging pipe and end salt discharging pipe are made up of Muscovitum.
According to an embodiment of the Molten salt chlorination furnace of production titanium tetrachloride of the present invention, described buffer fillings layer is made up of Graphite Powder 99, and fire brick layer is made up of alumino-silicate brick.
According to an embodiment of the Molten salt chlorination furnace of production titanium tetrachloride of the present invention, the opening for feed of described filling tube is higher than discharge port.
Molten salt chlorination furnace of the present invention in terms of existing technologies, has the following advantages: 1) fused salt chlorimation furnace body adopts three-decker, advantageously protects the shell of Molten salt chlorination furnace; 2) filling tube adopts the mode be obliquely installed, and feeds in raw material effective and prevents putty; 3) heating electrode and Chlorination tube there are the parts of leakproof chlorine, effectively can prevent the TiCl of chlorine and generation
4leak; 4) add bottom salt outlet simultaneously, effectively can discharge the abraum salt bottom chlorination furnace, the impurity component be deposited in production process bottom chlorination furnace is discharged chlorination furnace timely, effectively improve the molten salt nature in chlorination furnace.
Accompanying drawing explanation
Fig. 1 is the structural representation of the Molten salt chlorination furnace of the production titanium tetrachloride of exemplary embodiment of the present.
Description of reference numerals:
1-returns salt discharging pipe bottom ore pulp pipe, 2-filling tube, 3-metal furnace shell, 4-buffer fillings layer, 5-fire brick layer, 6-heating electrode, 7-electrode ear block, 8-Chlorination tube, 9-nozzle plug, 10-venting, 11 resultant mixing steam discharge ports, 12-salt discharge shutoff plug, 13-side salt discharging pipe, 14-fused salt, 15-thermopair, 16-pressure warning unit, 17-fused salt thermopair, 18-.
Embodiment
Below, the structure of the Molten salt chlorination furnace of the production titanium tetrachloride of exemplary embodiment of the present is described in detail with reference to accompanying drawing.
Fig. 1 is the structural representation of the Molten salt chlorination furnace of the production titanium tetrachloride of exemplary embodiment of the present.As shown in Figure 1, the top of the Molten salt chlorination furnace of production titanium tetrachloride of the present invention is arranged returns slurry pipe 1, filling tube 2, venting 10 and resultant mixing steam discharge port 11, wherein, filling tube 2 for adding the solid materials such as titanium slag in stove, the liquid fused salt of venting 10 for exhaust explosion and for adding high temperature, return slurry pipe 1 for spraying into the high liquid titanium tetrachloride of solid content when needing the temperature controlling fused salt in stove in stove, resultant mixing steam discharge port 11 generates titanium tetrachloride for discharging the reaction existed in a gaseous form and returns stove titanium tetrachloride, and the collection and aftertreatment that can directly carry out titanium tetrachloride product by being connected with collecting chamber by resultant mixing steam discharge port 11.Preferably, filling tube 2 is arranged with the angled manner of opening for feed higher than discharge port, feeds in raw material effective and prevents putty, convenient process.
The sidepiece of Molten salt chlorination furnace arranges side salt discharging pipe 13, many Chlorination tubes 8 and multiple heating electrode 6, wherein, side salt discharging pipe 12 in process of production timing discharge residue and abraum salt, Chlorination tube 8 reacts for passing into chlorine in stove, and heating electrode 6 is for heating fused salt 14.
Particularly, side salt discharging pipe 13 is also arranged salt discharge shutoff plug 12, after Molten salt chlorination furnace produces for some time, because residue and abraum salt increase in stove, need periodically to extract salt discharge shutoff plug 12 and carry out salt discharge operation.Preferably, side salt discharging pipe 13 is made up of Muscovitum, and salt discharge shutoff plug 12 is the conehead be made up of carbon steel.Protect the shutoff carrying out side salt discharging pipe 13 on salt discharge shutoff plug 12 with clay after salt discharge.
The outer wall of Chlorination tube 8 is arranged a circle nozzle plug 9 with gases did escape after preventing Chlorination tube 8 to be corroded.In one embodiment of the invention, be evenly arranged 4 Chlorination tubes at the sidepiece of Molten salt chlorination furnace, and Chlorination tube 8 insert and the bottom leading to fused salt 14 in stove to ensure that chlorine reacts with titanium slag equably.Preferably, Chlorination tube is made up of 2520 steel, but the present invention is not limited thereto.
Heating electrode 6 is Graphite Electrodes, and its one end connects power supply and the other end and to insert in stove in fused salt 14.In order to prevent gas from overflowing between heating electrode and furnace wall, the outside surface of heating electrode 6 arranges a circle electrode ear block 7.In one embodiment of the invention, Molten salt chlorination furnace comprises three heating electrodes 6, and these three heating electrodes are mutually hexagonal angle and arrange with the object reaching homogeneous heating.
The bottom of Molten salt chlorination furnace arranges end salt discharging pipe 18, and end salt discharging pipe 18 is for the bottom salt discharge of regular carrying out.Such as, when often producing one month, bottom salt discharge to be carried out to discharge the impurity composition being deposited in the difficult chlorination of fused salt chlorimation furnace bottom by bottom salt discharging pipe 18.The body of this end salt discharging pipe 18 is also made up of Muscovitum, and the salt discharge hole of end salt discharging pipe 18 is made up of carbon steel.During without the need to salt discharge, also with salt discharge shutoff plug (not shown), salt outlet is blocked anti-leak-stopping salt.
Comprise three layers according to the furnace wall of Molten salt chlorination furnace of the present invention, skin is metal furnace shell 3, and middle layer is buffer fillings layer 4, and internal layer is fire brick layer 5.Wherein, buffer fillings layer is made up of Graphite Powder 99, and because Graphite Powder 99 has character that is high temperature resistant, high strength, and thermal expansivity is little; the change of rapid heat cycle can be tolerated, so chlorination furnace temperature can be prevented in chlorination production process too high and affect the provide protection of chlorination furnace outer cover metal.Fire brick layer is made up of the alumino-silicate brick of acid-resistant and anti-high-temperature, and fire brick layer mainly prevents the corrosion of villaumite and chlorine, and isolates the large calorimetric of chlorination furnace reaction releasing, plays the effect of anticorrosion high temperature-proof, protection body of heater safety.
In order to the temperature and pressure of fused salt chlorimation furnace interior in Measurement accuracy production process, Molten salt chlorination furnace of the present invention also comprises the thermopair 15 and pressure warning unit 16 that are arranged at top, and is arranged at sidepiece to insert the fused salt thermopair 17 of fused salt in stove.Wherein, fused salt thermopair 17 comprises the pottery of outer field corundum and internal layer, is specifically designed to the temperature measuring fused salt.
The operation steps of the Molten salt chlorination furnace of production titanium tetrachloride of the present invention is illustrated below in conjunction with accompanying drawing.
A) will by NaCl and KCl be that the liquid fused salt that 7:3 forms is injected in Molten salt chlorination furnace from venting by a fused salt of two-maing ladle with mass ratio.By heating electrode, fused salt is heated to about 620 DEG C, wherein heating electrode is provided with the electrode ear block of graphite, heating electrode and electrode ear block are one, and electrode ear block can effectively prevent heating electrode and body of heater junction from losing heart.
B) by screw feeder, the compound be made up of titanium slag, refinery coke and sodium-chlor is sent in Molten salt chlorination furnace by filling tube.As the TiO of the fused salt in Molten salt chlorination furnace
2when content reaches 2 ~ 5%, C content reaches 3 ~ 5%, in Molten salt chlorination furnace, pass into chlorine by Chlorination tube, allow titanium slag and chlorine reaction produce TiCl
4.
C) because chlorination reaction process is exothermic process, therefore the temperature of molten salt in Molten salt chlorination furnace can raise, and temperature of molten salt is indicated by fused salt thermopair, is preferably controlled between 740 ~ 780 DEG C by temperature of molten salt.In order to control the temperature of fused salt well, must by returning ore pulp pipe the liquid TiCl admittedly containing object height
4spray in Molten salt chlorination furnace, reached the object of the temperature controlling Molten salt chlorination furnace by the temperature reducing fused salt.
D) TiCl that reaction is raw
4with the TiCl returning stove
4the following apparatus dust chamber of chlorination furnace is entered in the form of a vapor by resultant mixing steam discharge port.
In sum, the Molten salt chlorination furnace of production titanium tetrachloride of the present invention is adopted can to process the titanium slag raw material of high contents of calcium and magnesium content, to the thick TiCl of high solids content
4treatment capacity larger and effectiveness comparison good, the low and waste gas of chlorination temperature easily processes, and the titanium slag be particularly suitable for PZH vanadic-titanomagnetite is produced carries out TiCl
4production.Device structure is simple, anti-gas-leak, regularly can discharge abraum salt and improve chlorination environment, being conducive to TiCl
4production.
Although illustrate and describe the Molten salt chlorination furnace of production titanium tetrachloride of the present invention above in conjunction with the embodiments, but what those skilled in the art will appreciate that is, when not departing from the spirit and scope of the present invention as claims restriction, the various changes in form and details can be made here.
Claims (9)
1. produce the Molten salt chlorination furnace of titanium tetrachloride for one kind, it is characterized in that, the top of described Molten salt chlorination furnace is arranged returns slurry pipe, filling tube, venting and resultant mixing steam discharge port, the sidepiece of described Molten salt chlorination furnace arranges side salt discharging pipe, many Chlorination tubes and multiple heating electrode, the bottom of described Molten salt chlorination furnace arranges end salt discharging pipe, and the furnace wall of described Molten salt chlorination furnace comprises three layers, wherein, skin is metal furnace shell, middle layer is buffer fillings layer, internal layer is fire brick layer, the outer wall of described Chlorination tube is arranged a circle nozzle plug, the outside surface of described heating electrode arranges a circle electrode ear block.
2. the Molten salt chlorination furnace of production titanium tetrachloride according to claim 1, is characterized in that, described Molten salt chlorination furnace also comprises the thermopair and pressure warning unit that are arranged at top, and is arranged at sidepiece to insert the fused salt thermopair of fused salt in stove.
3. the Molten salt chlorination furnace of production titanium tetrachloride according to claim 2, is characterized in that, described fused salt thermopair comprises the pottery of outer field corundum and internal layer.
4. the Molten salt chlorination furnace of production titanium tetrachloride according to claim 1, is characterized in that, one end of described heating electrode connects power supply and the other end to insert in stove in fused salt.
5. the Molten salt chlorination furnace of production titanium tetrachloride according to claim 1, is characterized in that, described Molten salt chlorination furnace comprises three heating electrodes, and described three heating electrodes are mutually hexagonal angle and arrange.
6. the Molten salt chlorination furnace of production titanium tetrachloride according to claim 1, is characterized in that, described Molten salt chlorination furnace comprises four Chlorination tubes, and described Chlorination tube inserts and leads to the bottom of fused salt in stove.
7. the Molten salt chlorination furnace of production titanium tetrachloride according to claim 1, is characterized in that, described side salt discharging pipe and end salt discharging pipe also comprise salt discharge shutoff plug, and side salt discharging pipe and end salt discharging pipe are made up of Muscovitum.
8. the Molten salt chlorination furnace of production titanium tetrachloride according to claim 1, is characterized in that, described buffer fillings layer is made up of Graphite Powder 99, and fire brick layer is made up of alumino-silicate brick.
9. the Molten salt chlorination furnace of production titanium tetrachloride according to claim 1, is characterized in that, the opening for feed of described filling tube is higher than discharge port.
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| CN201310604232.3A CN103626224B (en) | 2013-11-25 | 2013-11-25 | Fused salt chlorination furnace for producing titanium tetrachloride |
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| CN103626224B true CN103626224B (en) | 2015-07-22 |
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| CN104198654B (en) * | 2014-08-15 | 2015-09-16 | 攀钢集团攀枝花钢铁研究院有限公司 | Fused salt chlorimation method produces the decision method of molten salt composition in titanium tetrachloride process |
| CN104591270A (en) * | 2015-01-28 | 2015-05-06 | 攀钢集团钛业有限责任公司 | Method for producing TiCl4 by using low-TiO2-grade titanium slag |
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| CN113932614B (en) * | 2021-10-31 | 2024-09-10 | 甘肃德通国钛金属有限公司 | Air inlet system of chlorination furnace and control method |
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| CN114353533B (en) * | 2022-01-14 | 2024-03-19 | 哈尔滨工程大学 | Salt discharging device at bottom of molten salt oxidation furnace and application method thereof |
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