CN105329940B - Method for preparing titanium tetrachloride from ultrafine-grained water quenching carbide slag - Google Patents
Method for preparing titanium tetrachloride from ultrafine-grained water quenching carbide slag Download PDFInfo
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- CN105329940B CN105329940B CN201510793846.XA CN201510793846A CN105329940B CN 105329940 B CN105329940 B CN 105329940B CN 201510793846 A CN201510793846 A CN 201510793846A CN 105329940 B CN105329940 B CN 105329940B
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- C01—INORGANIC CHEMISTRY
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- C01G23/00—Compounds of titanium
- C01G23/02—Halides of titanium
- C01G23/022—Titanium tetrachloride
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Abstract
The invention discloses a method for preparing titanium tetrachloride from ultrafine-grained water quenching carbide slag and aims to solve the problems that the ultrafine-grained carbide slag cannot be normally fluidized and heat release of the carbide slag reaction is intense. The method comprises steps as follows: quartz sand assisting in sulfuration is added to the ultrafine-grained water quenching carbide slag, all ultrafine-grained water quenching carbide slag can pass through a screen with the mesh number not smaller than 200, the titanium element in the ultrafine-grained water quenching carbide slag is extracted in a low-temperature chlorination mode, and titanium tetrachloride is produced. According to the method, the problem that the chlorination reaction effect is influenced due to overlarge heat release amount of chlorination reaction after wearing of the carbide slag is solved, and the chlorination ratio of titanium carbide in the carbide slag is increased and is higher than 95%.
Description
Technical field
Embodiments of the present invention are related to low-temperature boiling chlorination reaction technical field, more specifically, the embodiment party of the present invention
Formula is related to a kind of method for producing titanium tetrachloride using ultra-fine grade water quenching carbide slag.
Background technology
At present, the carbide slag that domestic low temperature chlorination is used is mainly slow cooling slag, and its type of cooling is to expose in atmosphere certainly
So cool down, be internally formed larger titanium carbide granule.As titanium carbide density and hardness is very big, its hardness exceedes diamond,
Break honed journey very difficult, it is difficult to reach 60 mesh～180 mesh needed for high-quality fluidization.
Through research, a kind of production decision of water quenching carbide slag is currently formed, hardness can be obtained in this way relatively low
Carbide slag.But, which sacrifices the size of titanium carbide granule, and the titanium carbide granule size inside carbide slag is less.If
The granule of water quenching carbide slag is excessive, then partially carbonized titanium granule cannot be exposed to its surface, cannot react in production
Generate titanium tetrachloride.Therefore, can be by not less than 200 purposes by water quenching carbide slag broken ultra-fine grade, i.e. the water quenching carbide slag of being ground to
Screen cloth, makes titanium carbide granule be sufficiently exposed to carbide slag surface.
But, superfine carbide slag is not suitable for fluidization production.Simultaneously as titanium carbide exposure is excessively fully, with chlorine
Gas contact area is larger, will cause that localized heat release amount is excessive, and temperature drastically increases, and is unfavorable for that fluidization is reacted.
The content of the invention
Instant invention overcomes the deficiencies in the prior art, there is provided a kind of to produce titanium tetrachloride using ultra-fine grade water quenching carbide slag
Method, to expect to solve, water quenching carbide slag grain diameter is too small, titanium carbide chlorination reaction thermal discharge is excessive to fluidization
The problem that reaction has a negative impact.
To solve above-mentioned technical problem, one embodiment of the present invention is employed the following technical solutions：
A kind of method for producing titanium tetrachloride using ultra-fine grade water quenching carbide slag, concrete operation step is：To superfine granule
The quartz sand of auxiliary sulfuration is added in level water quenching carbide slag, the ultra-fine grade water quenching carbide slag all can be not little by mesh number
In the screen cloth of 200 mesh, titanium elements therein are extracted by the way of 400～450 DEG C of low temperature chlorinations, generate titanium tetrachloride.
It is above-mentioned to be produced in the method for titanium tetrachloride using ultra-fine grade water quenching carbide slag, the ultra-fine grade water quenching carbide slag
It is that blast furnace slag carries out water quenching Jing after electric furnace carbonization when slagging tap, then is galled with ball mill and obtained；Wherein valuable constituent titanium carbide matter
Amount content is 12%～14%, and heap density is 1.1～1.3t/m3。
It is above-mentioned to be produced in the method for titanium tetrachloride using ultra-fine grade water quenching carbide slag, the granularity of the quartz sand 80～
It is in normal distribution between 140 mesh.
It is above-mentioned to be produced in the method for titanium tetrachloride using ultra-fine grade water quenching carbide slag, 400～450 DEG C of low temperature chlorinations
Concrete operations be：The compound of quartz sand and ultra-fine grade water quenching carbide slag is added in the furnace bottom of straight barrel type chlorination furnace, and is led to
Enter the fluidized gas comprising chlorine, in 400～450 DEG C of reactions of conversion zone temperature, make the titanium elements in ultra-fine grade water quenching carbide slag
It is chlorinated.
Above-mentioned to be produced in the method for titanium tetrachloride using ultra-fine grade water quenching carbide slag, the charging rate of the quartz sand is
3～4t/h, the charging rate of the ultra-fine grade water quenching carbide slag is 3～4t/h, and the mass flow of the chlorine accounts for superfine granule
The 25～30% of level water quenching carbide slag feeding quantity.
Above-mentioned to be produced in the method for titanium tetrachloride using ultra-fine grade water quenching carbide slag, the superficial gas velocity of the fluidized gas is
0.25～0.35m/s, in addition to chlorine, the fluidized gas needed for remaining are supplemented by nitrogen.
Above-mentioned to be produced in the method for titanium tetrachloride using ultra-fine grade water quenching carbide slag, the bed depth of the compound is
1.5～2.0m.
It is above-mentioned to be produced in the method for titanium tetrachloride using ultra-fine grade water quenching carbide slag, the deslagging of the straight barrel type chlorination furnace
Mouth is discharged from slag-drip opening in bed of material top, quartz sand.
Below technical scheme is further detailed.
The chlorination furnace that the present invention is used is straight barrel type, is not provided with expanding reach, it is therefore intended that promote the carbide slag after chlorination
Grain leaves chlorination furnace in being mixed in product gas.
Carbonization solid impurity particle is broken and is ground to the screen cloth that all can be not less than 200 mesh by mesh number, it is therefore an objective to fully exposed which and contain
Some valuable constituent titanium carbides, promote the generation chlorination reaction of more than 95% titanium carbide to generate titanium tetrachloride.
Quartz sand size is in normal distribution between 80 mesh～140 mesh, plays the fluidised effect of auxiliary and absorbing reaction
The effect of heat.Slag-drip opening of the quartz sand from the top of the bed of material is discharged, according to about 1 after cooling:1 ratio is mixed with water quenching carbide slag,
Then add in stove from chlorination furnace bottom, realize recycling.
The chlorination furnace bed of material control in 1.5～2.0m, it is ensured that the titanium carbide in compound from furnace bottom run up furnace roof when,
React complete in theory, i.e. titanium carbide chlorination rate reaches more than 95%.
The superficial gas velocity of chlorination furnace is 0.25～0.35m/s, and under here gas speed, the bed of material is obtained in that
Amount, and can guarantee that reacted carbonization solid impurity particle elutriation leaves.Further, since there is certain matching in carbide slag feeding quantity and chlorine
Relation, fluidized gas insufficient section use nitrogen.
Compared with prior art, one of beneficial effects of the present invention are：It is anti-that the present invention solves carbide slag worn-off afterchlorinate
The excessive problem for affecting chlorination reaction effect of thermal discharge is answered, the chlorination rate of titanium carbide in carbide slag is increased, is reached chlorination rate
More than 95%.
Description of the drawings
Fig. 1 is the flow chart of the method that the present invention produces titanium tetrachloride using ultra-fine grade water quenching carbide slag.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, it is below in conjunction with drawings and Examples, right
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only to explain the present invention, and
It is not used in the restriction present invention.
As shown in figure 1, the present invention is obtained through low temperature chlorination and cyclone dust collection after water quenching carbide slag is mixed with quartz sand
Product gas (titanium tetrachloride) and chloride residue, the chlorination furnace for using are straight barrel type chlorination furnaces, and the slag-drip opening of chlorination furnace is on the bed of material
Portion, quartz sand are cooled down from after slag-drip opening discharge, and the quartz sand after cooling is recycled.
Embodiment 1
Blast furnace slag is carried out into water quenching Jing after electric furnace carbonization when slagging tap, then is milled to ball mill that all to pass through mesh number not little
In the screen cloth of 200 mesh；Wherein valuable constituent titanium carbide mass content is about 13%, and heap density is about 1.1.2t/m3, obtain ultra-fine
Grade water quenching carbide slag.Quartz sand is crushed, keeps its granularity to be in normal distribution between 80～140 mesh.Then by superfine granule
Level water quenching carbide slag is with quartz sand according to mass ratio 1:1 mix homogeneously, obtains compound.The compound is added to into straight barrel type chlorine
Change the furnace bottom of stove, the bed depth of compound is 1.5m, wherein, the charging rate of quartz sand is 3.5t/h, ultra-fine grade water quenching
Carbide slag is same, therefore the charging rate of above-mentioned compound is sum of the two, i.e. 7t/h.Apparent gas is passed through in chlorination furnace
Fluidized gas of the speed for 0.25～0.35m/s, fluidized gas are made up of chlorine and nitrogen, and the mass flow of chlorine accounts for ultra-fine grade water quenching
The 28% of carbide slag feeding quantity, remaining gas are nitrogen.Titanium elements in ultra-fine grade water quenching carbide slag are with chlorine in conversion zone
(400～450 DEG C) reactions obtain titanium tetrachloride.The chlorination rate of titanium carbide is 96.5%.
Embodiment 2
Blast furnace slag is carried out into water quenching Jing after electric furnace carbonization when slagging tap, then is milled to ball mill that all to pass through mesh number not little
In the screen cloth of 200 mesh；Wherein valuable constituent titanium carbide mass content is about 14%, and heap density is about 1.3t/m3, obtain superfine granule
Level water quenching carbide slag.Quartz sand is crushed, keeps its granularity to be in normal distribution between 80～140 mesh.Then by ultra-fine grade
Water quenching carbide slag is with quartz sand according to mass ratio 1:1 mix homogeneously, obtains compound.The compound is added to into straight barrel type chlorination
The furnace bottom of stove, the bed depth of compound is 2.0m, wherein, the charging rate of quartz sand is 4t/h, ultra-fine grade water quenching carbonization
Slag is same, therefore the charging rate of above-mentioned compound is sum of the two, i.e. 8t/h.To in chlorination furnace being passed through superficial gas velocity is
The fluidized gas of 0.25～0.35m/s, fluidized gas are made up of chlorine and nitrogen, and the mass flow of chlorine accounts for ultra-fine grade water quenching carbonization
The 30% of slag feeding quantity, remaining gas are nitrogen.Titanium elements in ultra-fine grade water quenching carbide slag are with chlorine in conversion zone (400
～450 DEG C) reaction acquisition titanium tetrachloride.The chlorination rate of titanium carbide is 95.5%.
Embodiment 3
Blast furnace slag is carried out into water quenching at 1600 DEG C Jing after electric furnace carbonization when slagging tap, then is milled to ball mill and can all be passed through
Screen cloth of the mesh number not less than 200 mesh；Wherein valuable constituent titanium carbide mass content is about 12%, and heap density is about 1.1t/m3, obtain
To ultra-fine grade water quenching carbide slag.Quartz sand is crushed, keeps its granularity to be in normal distribution between 80～140 mesh.Then will
Ultra-fine grade water quenching carbide slag is with quartz sand according to mass ratio 1:1 mix homogeneously, obtains compound.The compound is added to directly
The furnace bottom of cartridge type chlorination furnace, the bed depth of compound are 1.8m, wherein, the charging rate of quartz sand is 3t/h, ultra-fine grade
Water quenching carbide slag is same, therefore the charging rate of above-mentioned compound is sum of the two, i.e. 3t/h.Table is passed through in chlorination furnace
Fluidized gas of the gas speed for 0.25～0.35m/s are seen, fluidized gas are made up of chlorine and nitrogen, and the mass flow of chlorine accounts for ultra-fine grade
The 25% of water quenching carbide slag feeding quantity, remaining gas are nitrogen.Titanium elements in ultra-fine grade water quenching carbide slag are with chlorine anti-
(400～450 DEG C) reactions of section are answered to obtain titanium tetrachloride.The chlorination rate of titanium carbide is 96%.
Although reference be made herein to invention has been described for explanatory embodiment of the invention, however, it is to be understood that ability
Field technique personnel can be designed that a lot of other modifications and embodiment, and these modifications and embodiment will fall in the application public affairs
Within the spirit opened and spirit.More specifically, in the range of disclosure, can be to the group of theme composite configuration
Various modifications and improvement are carried out into part and/or layout.Except the modification that carries out to building block and/or layout and in addition to improving,
To those skilled in the art, other purposes also will be apparent.
Claims (7)
1. it is a kind of using ultra-fine grade water quenching carbide slag produce titanium tetrachloride method, it is characterised in that to ultra-fine grade water quenching carbon
Add the quartz sand of auxiliary fluidisation, the ultra-fine grade water quenching carbide slag all can be not less than 200 mesh by mesh number in slugging
Screen cloth, the granularity of the quartz sand is in normal distribution between 80～140 mesh, by the way of 400～450 DEG C of low temperature chlorinations
Titanium elements therein are extracted, titanium tetrachloride is generated.
2. it is according to claim 1 using ultra-fine grade water quenching carbide slag produce titanium tetrachloride method, it is characterised in that
The ultra-fine grade water quenching carbide slag is that blast furnace slag carries out water quenching Jing after electric furnace carbonization when slagging tap, then with ball mill worn-off
；Wherein valuable constituent titanium carbide mass content is 12%～14%, and heap density is 1.1～1.3t/m3。
3. it is according to claim 1 using ultra-fine grade water quenching carbide slag produce titanium tetrachloride method, it is characterised in that
The concrete operations of 400～450 DEG C of low temperature chlorinations are：Quartz sand and ultra-fine grade water are added in the furnace bottom of straight barrel type chlorination furnace
Quench the compound of carbide slag, and be passed through the fluidized gas comprising chlorine, in 400～450 DEG C of reactions of conversion zone temperature, make ultra-fine grade
Titanium elements in water quenching carbide slag are chlorinated.
4. it is according to claim 3 using ultra-fine grade water quenching carbide slag produce titanium tetrachloride method, it is characterised in that
The charging rate of the quartz sand is 3～4t/h, and the charging rate of the ultra-fine grade water quenching carbide slag is 3～4t/h, described
The mass flow of chlorine accounts for the 25～30% of ultra-fine grade water quenching carbide slag feeding quantity.
5. it is according to claim 4 using ultra-fine grade water quenching carbide slag produce titanium tetrachloride method, it is characterised in that
The superficial gas velocity of the fluidized gas is 0.25～0.35m/s, and in addition to chlorine, the fluidized gas needed for remaining are supplemented by nitrogen.
6. it is according to claim 3 using ultra-fine grade water quenching carbide slag produce titanium tetrachloride method, it is characterised in that
The bed depth of the compound is 1.5～2.0m.
7. it is according to claim 6 using ultra-fine grade water quenching carbide slag produce titanium tetrachloride method, it is characterised in that
The slag-drip opening of the straight barrel type chlorination furnace is discharged from slag-drip opening in bed of material top, quartz sand.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105905939B (en) * | 2016-04-21 | 2017-07-28 | 重庆大学 | The apparatus and method of chlorination are directly granulated after a kind of titanium-containing blast furnace slag carbonization |
| CN106269173B (en) * | 2016-10-09 | 2018-06-12 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of breaking method of carbide slag |
| CN107601555A (en) * | 2017-10-26 | 2018-01-19 | 攀钢集团攀枝花钢铁研究院有限公司 | Carbide slag fluidizes chlorination |
| CN114426304B (en) * | 2020-10-29 | 2023-05-12 | 中国科学院过程工程研究所 | Method for extracting titanium from titanium carbide slag by fluidization low-temperature chlorination |
| CN114162855A (en) * | 2021-12-16 | 2022-03-11 | 朝阳百盛钛业股份有限公司 | Technology for slag discharge and slag water quenching without stopping chlorine in boiling chlorination |
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| CN1033264A (en) * | 1987-10-27 | 1989-06-07 | 冶金工业部攀枝花钢铁公司钢铁研究院 | The method of preparing titanic chloride using carbon-containing slag |
| CN103816963A (en) * | 2014-03-03 | 2014-05-28 | 攀钢集团攀枝花钢铁研究院有限公司 | Carbide slag grinding method and low temperature chlorination method for preparing TiCl4 |
| CN104646111A (en) * | 2015-03-05 | 2015-05-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Water quenching carbonized dreg grinding method |
| CN103480306B (en) * | 2013-09-06 | 2015-10-14 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method of low-temperature boiling chlorination furnace and production titanium tetrachloride |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2013100048A1 (en) * | 2011-12-27 | 2013-07-04 | 石原産業株式会社 | Titanium dioxide granules for use in production of titanium tetrachloride, and method for producing same |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1033264A (en) * | 1987-10-27 | 1989-06-07 | 冶金工业部攀枝花钢铁公司钢铁研究院 | The method of preparing titanic chloride using carbon-containing slag |
| CN103480306B (en) * | 2013-09-06 | 2015-10-14 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method of low-temperature boiling chlorination furnace and production titanium tetrachloride |
| CN103816963A (en) * | 2014-03-03 | 2014-05-28 | 攀钢集团攀枝花钢铁研究院有限公司 | Carbide slag grinding method and low temperature chlorination method for preparing TiCl4 |
| CN104646111A (en) * | 2015-03-05 | 2015-05-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Water quenching carbonized dreg grinding method |
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