CN1033264A - The method of preparing titanic chloride using carbon-containing slag - Google Patents
The method of preparing titanic chloride using carbon-containing slag Download PDFInfo
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- CN1033264A CN1033264A CN 87107488 CN87107488A CN1033264A CN 1033264 A CN1033264 A CN 1033264A CN 87107488 CN87107488 CN 87107488 CN 87107488 A CN87107488 A CN 87107488A CN 1033264 A CN1033264 A CN 1033264A
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Abstract
The method of preparing titanic chloride using carbon-containing slag, the byproduct that is a kind of processing blast-furnace smelting titanium magnet ore concentrate (or v-ti magnetite concentrate) is the method for preparing titanic chloride using carbon-containing slag.The content of titanium dioxide of blast furnace slag is 15-35%.Liquid blast furnace flows into the closed electric furnace and carries out carbonization, and carbonation rate can reach more than 90%.Carbonization blast furnace slag low temperature chlorination in fluidized-bed, chlorination rate is greater than 85%.
Description
The invention belongs to and handle titaniferous metallurgical slag producing titanium tetrachloride t 5 bx method and technology field, the byproduct that is particularly suitable for handling blast-furnace smelting titanium magnet ore concentrate (or v-ti magnetite concentrate) is a preparing titanic chloride using carbon-containing slag.
The solid metallurgical slag that New Zealand once will contain ferrous oxide about 33% is reductive agent with carbon, makes the nitrogenize of titanium reduction carbon in the tunnel kiln under 1350 ℃ of-1400 ℃ of temperature.The iron blast furnace slag that contains after the carbon nitrogenize is produced titanium tetrachloride through low temperature chlorination.Also there is similar method in the U.S..This method is that cold slag fine grinding, height join that the carbon stove mixes outward, indirect heating reduction carbon nitrogenize in the tunnel kiln.The shortcoming of these methods is that long flow path, carbon nitrogenizing reaction speed are slow, material is all low in kiln residence time length, thermo-efficiency and production efficiency, is difficult to realize commercial production.
US3,899,569 United States Patent (USP)s add an amount of calcium oxide when the electrosmelting ilmenite, the temperature of smelting titanic iron ore is decreased, and operation makes moderate progress.The above-mentioned titanium slag that contains calcium oxide is mixed the carbon of sufficient amount, in single-phase arc funace, under a little more than 1850 ℃ of temperature, make titanium dioxide and calcium oxide all generate carbide.On the top of the slag, use the carbon dust covering protection at the stove internal cooling.Cold slag that takes out and water reaction, its carbide of calcium resolves into acetylene and calcium hydroxide, and the titanium carbide particulate of disperse in the carbide of calcium matrix is released among the ore pulp that is scattered in calcium hydroxide.According to the difference of proportion, select the titanium carbide concentrate with gravity separation method.The titanium carbide concentrate is the chlorination producing titanium tetrachloride t 5 bx under 225 ℃-300 ℃ temperature.As long as uhligite is joined enough carbon, with aforesaid method carbonization, chlorination, producing titanium tetrachloride t 5 bx.The titaniferous thing that this method is handled, content of titanium dioxide is all greater than 50%, and SiO
2, Al
2O
3With MgO percentage composition separately all less than 5%.Its shortcoming is:
1. cold slag is gone into the stove carbonization, the power consumption height.
2. the requirement of carbon is many, is the 110-150% that calcium oxide and titanium dioxide generate carbide separately and carbon monoxide theoretical amount simultaneously.
3. slag can not be emitted outside the stove after the carbonization, needs under the carbon dust protection at the stove internal cooling, reoxidizes in order to avoid contact with air, and the carbonization electric furnace can not carry out continuous production, and plant factor and productivity are low.
4. cold slag takes out fragile furnace lining in the carbonization electric furnace.
Therefore, be difficult to carry out commercial production.To content of titanium dioxide 24-35% only, and SiO
2, Al
2O
3With MgO content summation up to 45% to 35% blast furnace slag, US3,899,569 United States Patent (USP)s can not effectively be handled.
The objective of the invention is to make improvements at the problems referred to above, propose a kind of liquid Fe-contg blast furnace slag and flow into the closed electric furnace the blast furnace discharging, carry out carbonization in stove under the high temperature, the carbonization blast furnace slag carries out the method for chlorating producing titanium tetrachloride t 5 bx under the low temperature in fluidized-bed.It is low to handle content of titanium dioxide in this way, and SiO
2, Al
2O
3With the high blast furnace slag of MgO content summation.Again because this method energy consumption is low, flow process is short, production efficiency is high, so production cost is low, can carry out commercial production.
The method that this iron content blast furnace slag is produced titanium tetrachloride is to make the reaction of blast furnace slag and carbon carry out the carbonization blast furnace slag and chlorine reaction carries out chlorination.Content of titanium dioxide only has 15-35% in the handled blast furnace slag, and SiO
2, Al
2O
3, MgO, CaO equal size summation reach more than 65%.The liquid titanium-containing blast furnace slag of blast furnace discharging is flowed into the closed electric furnace, in stove, add carbon and carry out carbonization.The carbon add-on is the 110-120% that the titanium dioxide reaction generates titanium carbide and carbon monoxide stoichiometric calculation theoretical amount in carbon and the slag.The temperature of reaction of carbonation reaction is 1600 ℃-1800 ℃.Blast furnace slag after the carbonization is in a liquid state and emits from the closed electric furnace, cools off in air, and cooling is after broken, fine grinding becomes particulate state.Granular carbonization blast furnace slag is used chlorinated with chlorine in fluidized-bed.The temperature of reaction of chlorination reaction process should remain between 250 ℃-600 ℃.
The iron level of handled blast furnace slag is less than 5% in metal, otherwise, not only reduced the iron productivity of blast-furnace smelting, and when carbonization, generated the consumption that iron carbide has increased carbon, when chlorination, increased the consumption of chlorine again, generated more and the little iron trichloride of use.The closed electric furnace make liquid blast furnace in carbonization process not with or seldom contact with air, avoid air invade to increase the consumption of carbon and produce thermal convection carbon dust taken away in a large number, guarantee the sound response of liquid blast furnace and carbon.
CaO, MgO, SiO in the liquid blast furnace
2, Al
2O
3Weight percent to obey following relational expression:
Guarantee after titanium dioxide is carbonized, to transfer to and SiO with titanium dioxide bonded CaO, MgO in the original slag
2, Al
2O
3In conjunction with generating 2CaOMgO2SiO
2Or 2CaOAl
2O
3SiO
2And so on the silicate and the glassiness.The viscosity of liquid blast furnace that contains these materials is less, and the CO gas that helps reacting generation stirs in slag and overflows.Stirring has promoted mixing of liquid blast furnace and carbon, and good reacting dynamics condition is provided.These materials are difficult for chlorination in the low temperature chlorination reaction process, thereby have improved the effective rate of utilization of chlorine.
Chlorination temperature remain on 400 ℃-550 ℃ more favourable to chlorination process.Temperature of reaction speed of response between 250 ℃-400 ℃ is slow, and the chlorination rate of titanium is than corresponding low (＜85%) more than 400 ℃ in the same reaction times.In addition, the titanium tetrachloride vapors that generates between 250 ℃-400 ℃ is easy to cool off because of dissipated heat in the effusion process.Therefore, the condensation point that temperature is easy to drop to titanium tetrachloride makes the titanium tetrachloride condensation below 136 ℃, brings difficulty for the dedusting of later treating processes.Just can be if chlorination reaction temperature between 550 ℃-600 ℃, is operated careless slightly temperature above 600 ℃.When chlorination temperature was higher than 600 ℃, it is very fast that the chlorination rate of calcium, magnesium rises, and makes the material sintering easily and destroyed boiling state, makes the fluidized-bed can not ordinary production.So chlorination reaction temperature remains between 400 ℃-550 ℃ the most favourable.Because carbonization blast furnace slag titaniferous grade is very low, impurity is many, and very fast these characteristics of the speed of response of chlorine and titanium carbide are wanted the continuous charging continuous discharging slag in the chlorination reaction process in fluidized-bed.
Method of the present invention and US3,899,569 United States Patent (USP)s are compared, and save hydrolysis, gravity treatment two procedures.1420 ℃-1450 ℃ the titanium-containing slag that blast furnace is given off flows into the closed electric furnace, can make full use of slag physics heat, can be warming up to 1600 ℃-1800 ℃ as long as replenish a little heat, saves power consumption 40%, and equipment capacity improves 30%.The add-on of carbon is the 110-120% that generates titanium carbide and carbon monoxide theoretical amount, rather than United States Patent (USP) carbon add-on is the 110-150% that calcium oxide and titanium dioxide generate carbide separately and carbon monoxide theoretical amount simultaneously.The carbon that does not only generate carbide of calcium and consumed, and the per-cent of the actual requirement of carbon and theoretical amount is little.Can reach more than 90% with closed electric furnace carbonization blast furnace slag carbonation rate, the carbonation rate of United States Patent (USP) is 85%-90%.
Fluidized-bed is faster than fixed bed and moving-bed heat and mass, and temperature is even, and throughput is big.Prior art fluidized bed chlorination producing titanium tetrachloride t 5 bx all has strict restriction to the content of CaO in the chloride material and MgO, and the two resultant of generalized case can not surpass 10%(weight).Method of the present invention is quite different, as long as satisfy relational expression:
Titanium dioxide is reduced after the carbonization, and CaO chemically combined with it and MgO transfer SiO to
2And Al
2O
3In conjunction with generating complicated silicate, this class silicate is difficult to chlorination at low temperatures than simple oxidation calcium and magnesium oxide.And titanium carbide very easily chlorination at low temperatures, promptly titanium carbide has first chlorating advantage than this class silicate at low temperatures.The chlorination rate of titanium is greater than 85%, and content of titanium dioxide is less than 4% in the chloride residue of discharge, and the chlorination rate of calcium can be less than 7%, and the chlorination rate of magnesium can be less than 5%.The titanium chloride steam that reaction generates can obtain more purified liquid titanium tetrachloride through dedusting, condensation after overflowing.Wherein vanadium, silicon, aluminium, iron all can be removed by known technology.The titanium tetrachloride that current technology is produced all will could be produced titanium sponge or titanium white after refining, content of titanium dioxide after muriate is removed in water logging, can be made the raw material of cement baking less than 4% chloride residue, and titanium-containing blast furnace slag is fully used.
Method chlorination reaction temperature of the present invention is 250 ℃-600 ℃, and remain between 400 ℃-550 ℃ the most favourable, than U.S. Pat 3,899,225 ℃-300 ℃ high of 659 chlorination temperatures, and temperature range is big.Because chlorination reaction is a strong exothermic reaction, so the heat that the chlorination reaction process of United States Patent (USP) need be discharged is many, temperature of reaction is restive.Though iron trichloride impurity is more some more than United States Patent (USP) in the titanium tetrachloride vapors of method of the present invention, the liquid titanium tetrachloride of producing all will could be produced titanium sponge or titanium white through refining.
Accompanying drawing is seen in technical process of the present invention.Its master operation is as follows:
1. make 1420 ℃ of-1450 ℃ of liquid molten titanium-containing blast furnace slags of blast furnace discharging directly or indirectly flow into the closed electric furnace, carbon is sprinkled upon on the fusion titanium-containing blast furnace slag with the 110-120% with titanium dioxide generation titanium carbide and carbon monoxide theoretical amount in electric furnace, heat up 600 ℃-1800 ℃ and carry out carbonization, the blast furnace slag after the carbonization is in a liquid state and emits from closed electric furnace.
2. liquid carbonization blast furnace slag cools off in air, and cooling is after broken, fine grinding becomes particulate state.
3. the granular carbonization blast furnace slag seethes with excitement in aerodynamic condition with chlorine in fluidized-bed and contacts and chlorination, and chlorination reaction temperature must remain between 250 ℃-600 ℃, generates crude titanic chloride and chloride slag after the chlorination.
The fusion titanium-containing blast furnace slag of 150kg1420 ℃ of Panzhihua Iron blast-furnace smelting v-ti magnetite concentrate is packed in the 250KVA closed electric furnace, again with the 30.5kg hard coal on the slag face.Actual mixed carbon comtent is the 109-116% of theoretical mixed carbon comtent.Coal dust finishes immediately energising and heats up and carry out carburizing reagent, and temperature of reaction is after reaction in about 60 minutes finishes about 1700 ℃, promptly slags tap.Tapping temperature is 1600 ℃-1680 ℃, and the liquid carbide slag of emitting is contained in the inherent air of alloy slag ladle and cooled off.The carbonation rate average out to 91.5% of titanium, carbonization slag carbon containing titanium 16.7%, the ore deposit that other compositions form mainly is melilith mutually, secondly is the aluminum-spinel and the glassiness.
The steel climbing high slag Chemical Composition
| Chemical Composition | SiO 2 | V 2O 5 | TiO 2 | Al 2O 3 | CaO | MgO | TFe |
| Percentage composition % | 23.12 | 0.30 | 24.35 | 13.17 | 24.01 | 9.16 | 4.01 |
Climb steel carbonization blast furnace slag Chemical Composition
| Chemical Composition | SiO 2 | V 2O 5 | TiO * 2 | Al 2O 3 | CaO | MgO | TFe** | TiC |
| Percentage composition % | 25.76 | 0.29 | 24.18 | 15.16 | 25.56 | 9.90 | 2.90 | 16.70 |
* the Ti(CN in the carbide slag) and at a low price titanium is all amounted to into titanium dioxide and is counted.
The * metallic iron is heavy than slag, and bigger iron shot is sunken to the slag ladle bottom segregation, has selected when ore grinding.
Cooled carbonization blast furnace slag through broken, be finely ground to one 100～+ 200 orders and account for more than 65%, the pulverulent material of-200 orders＜35% is sent into fluidized-bed and is contacted with chlorine, carries out the chlorination reaction producing titanium tetrachloride t 5 bx under 400 ℃-550 ℃ temperature.Actual fluidizing gas velocity is 0.2m/s, and material is 30-60 minute at residing time in furnace, the continuous charging continuous discharging slag.The chlorination rate of titanium is greater than 85%, and the chlorination rate of calcium is less than 7%, and the chlorination rate of magnesium is less than 5%.Content of titanium dioxide is less than 4% in the chloride slag of discharging, and the chloride slag after the washing can be used as the raw material of cement baking.
Washing post chlorization dreg chemistry composition
| Chemical Composition | TiO 2 | SiO 2 | Al 2O 3 | CaO | MgO | TFe | V 2O 5 |
| Percentage composition % | 3.35 | 33.37 | 18.26 | 28.35 | 11.61 | 1.30 | 0.07 |
The molten iron of blast furnace smelting v-ti magnetite concentrate can extract vanadium slag and produce Vanadium Pentoxide in FLAKES, but the titanium-containing blast furnace slag producing titanium tetrachloride t 5 bx, but remaining residue stove system cement.Like this, the iron in the vanadium titano-magnetite, vanadium, titanium, the whole comprehensive reutilizations of residue, perfect whole technical process of v-ti magnetite concentrate.
Climb steel carbonization blast furnace slag in 600 ℃ of-800 ℃ of chlorination reaction process, the variation of calcium, magnesium chlorination rate is as follows:
| Chlorination temperature ℃ | ＜600℃ | ＞600℃ | About 700 ℃ | About 800 ℃ |
| Calcium chlorination rate % | ＜10 | ＞10 | ≈ 30(sintering) | ≈ 70(sintering) |
| Magnesium chlorination rate % | ＜5 | ＞5 | ≈ 10(sintering) | ≈ 30(sintering) |
This shows that chlorination temperature is during greater than 600 ℃, calcium, the increase of magnesium chlorination rate are very fast, and sintering can take place, thereby have destroyed the boiling state in the fluidized-bed, and fluidized-bed can not be produced.
Claims (3)
1, a kind of method of preparing titanic chloride using carbon-containing slag, comprising:
A) make blast furnace slag and carbon the reaction carry out carbonization and
B) make carbonization blast furnace slag and chlorine reaction carry out chlorination,
The invention is characterized in:
C) content of titanium dioxide is 15-35% in the blast furnace slag,
D) liquid blast furnace flows into the carbonization in stove of closed electric furnace,
E) the carbon add-on is the 110-120% that generates titanium carbide and carbon monoxide theoretical amount,
F) carbonation reaction temperature is 1600 ℃-1800 ℃,
G) fine grinding becomes the chlorination in fluidized-bed of granular carbonization blast furnace slag,
H) chlorination reaction temperature is 250 ℃-600 ℃.
2, by the said method of claim 1, it is characterized in that CaO in the liquid blast furnace, MgO, SiO
2And Al
2O
3Weight percent to obey following relational expression:
According to claim 1 or 2 said methods, it is characterized in that 3, chlorination reaction temperature is 400 ℃-550 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN87107488.5A CN1005629B (en) | 1987-10-27 | 1987-10-27 | Method for preparing titanium tetrachloride from titanium-containing blast furnace slag |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN87107488.5A CN1005629B (en) | 1987-10-27 | 1987-10-27 | Method for preparing titanium tetrachloride from titanium-containing blast furnace slag |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1033264A true CN1033264A (en) | 1989-06-07 |
| CN1005629B CN1005629B (en) | 1989-11-01 |
Family
ID=4816102
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN87107488.5A Expired CN1005629B (en) | 1987-10-27 | 1987-10-27 | Method for preparing titanium tetrachloride from titanium-containing blast furnace slag |
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