CN107601555A - Carbide slag fluidizes chlorination - Google Patents
Carbide slag fluidizes chlorination Download PDFInfo
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- CN107601555A CN107601555A CN201711014560.2A CN201711014560A CN107601555A CN 107601555 A CN107601555 A CN 107601555A CN 201711014560 A CN201711014560 A CN 201711014560A CN 107601555 A CN107601555 A CN 107601555A
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Abstract
The invention belongs to chemical metallurgy technical field, and in particular to a kind of carbide slag fluidizes chlorination.It is low for existing carbide slag chloridization process chlorination rate, the technical problem for causing chlorination furnace to cohere defluidization is also easy to, the present invention provides a kind of carbide slag fluidisation chlorination, comprised the following steps：A, carbonization solid impurity particle is put into fluid bed, is passed through chlorine and carries out chlorination reaction, chlorination reaction temperature is 400~650 DEG C, and the chlorination reaction time is 1~10min；B, by the mixture obtained by step a after titanium tetrachloride elution circuit elutes and cools down, the titanium tetrachloride of isolated chlorine and liquid.The present invention carries out chlorination by using fast fluidized bed to carbide slag, and heat and mass is fast, and Chlorination speed is fast, and can effectively avoid fluid bed coheres defluidization problem, while can also recycle chlorine and carbide slag, saves production cost.
Description
Technical field
The invention belongs to chemical metallurgy technical field, and in particular to a kind of carbide slag fluidizes chlorination.
Background technology
China is the country that titanium resource is most abundant in the world, and explored titanium ore reserves account for the 48% of world's total amount.China
Titanium resource is mainly based on the vanadium titano-magnetite of Panxi Diqu, but this ilmenite is a kind of typical complicated pluralism element rock ore deposit,
Its TiO2Grade is low, and its calcium and magnesium impurity content is high, reaches 7~11%, caused high calcium after this v-bearing titanomagnetite smelting
Magnesium high-titanium blast furnace slag is not used to the existing chloridization process for having sieve plate boiling chloridizing furnace.
For this special titanium mineral, using " blast furnace slag high temperature cabonization-cryogenic selective chlorination-titanium extraction tailings integrate profit
With " process route can obtain the utilization of industrialization.The high temperature cabonization technique is high with carbonaceous reducing agent at high temperature
Titanium blast furnace slag, TiC content is 11~15% in obtained carbide slag.The low temperature chlorination refers to use at 500~550 DEG C
Chlorine is by the titanium carbide chlorination obtained by high temperature cabonization technique into titanium tetrachloride.But no matter titanium carbide have oxi-chlorination or
Without oxi-chlorination, substantial amounts of heat will be all released, if not in time taking away heat, can make it that local temperature in chlorination furnace is higher,
Reach the chlorination temperature of calcium oxide and magnesia, so as to which cause chlorination furnace coheres defluidization.In existing low temperature chlorination technique, it is
Raising chlorination efficiency, typically by increasing residence time of the carbide slag in chlorination furnace or improving chlorination reaction temperature come complete
Into, but these measures can all increase the probability that chlorination furnace coheres defluidization.A kind of new carbide slag chlorination is urgently developed at present,
While to ensure chlorination efficiency, the probability for cohering defluidization of chlorination furnace is reduced.
The content of the invention
The technical problem to be solved in the present invention is：Existing carbide slag chloridization process chlorination rate is low, is also easy to cause chlorination
Stove coheres the technical problem of defluidization.
The present invention solve technical problem technical scheme be：A kind of carbide slag fluidisation chlorination is provided.This method includes
Following steps：
A, will carbonization solid impurity particle be put into fluid bed, be passed through chlorine carry out chlorination reaction, chlorination reaction temperature be 400~
650 DEG C, the chlorination reaction time is 1~10min；
B, by the mixture obtained by step a after titanium tetrachloride elution circuit elutes and cools down, isolated chlorine and liquid
The titanium tetrachloride of state.
Wherein, in above-mentioned carbide slag fluidisation chlorination, carbide slag described in step a is TiC contents 11~15%, oxidation
Silicone content 25~29%, calcium oxide content 24~28%, content of magnesia 7~10%, alumina content 12~14%, carbon content
7~9%, surplus is the carbide slag of impurity.
Wherein, in above-mentioned carbide slag fluidisation chlorination, carbide slag particle diameter described in step a is 80~800 mesh, preferably
120~400 mesh.
Wherein, in above-mentioned carbide slag fluidisation chlorination, the draw ratio of fluidized bed chlorination section described in step a is 20~
30:1。
Wherein, in above-mentioned carbide slag fluidisation chlorination, the flow velocity that chlorine is passed through in step a is 2~6m/s.
Wherein, in above-mentioned carbide slag fluidisation chlorination, the purity of chlorine gas feeding being passed through described in step a is 60~80%.
Wherein, in above-mentioned carbide slag fluidisation chlorination, lessivation is described in step b：Gas temperature by 450~
430 DEG C drop to 0~-5 DEG C by three-level elution, titanium tetrachloride yield >=98%.
Wherein, in above-mentioned carbide slag fluidisation chlorination, chlorine described in step b and the equal return to step a institutes of titanium tetrachloride
State in fluid bed and recycle.
Compared with prior art, beneficial effects of the present invention are：The invention provides a kind of carbide slag to fluidize chlorination,
Chlorination is carried out to carbide slag by using fast fluidized bed, heat and mass is fast, and Chlorination speed is fast, can effectively avoid the glutinous of fluid bed
Tie defluidization problem；The inventive method carbide slag rate of recovery is high simultaneously, and unnecessary chlorine and carbide slag may continue to return after reaction
Return fluid bed and continue chlorination, raw material availability has obvious economic benefit up to 100%.The inventive method not only increases
The rate of recovery of carbide slag, it is thus also avoided that chlorination furnace coheres defluidization problem, and economic benefit is obvious, suitably promotes the use of.
Embodiment
The invention provides a kind of carbide slag to fluidize chlorination, comprises the following steps：
A, will carbonization solid impurity particle be put into fluid bed, be passed through chlorine carry out chlorination reaction, chlorination reaction temperature be 400~
650 DEG C, the chlorination reaction time is 1~10min；
B, after the mixed material obtained by step a being eluted and cooled down by titanium tetrachloride elution circuit, liquid tetrachloro is obtained
Change titanium.
Wherein, in above-mentioned carbide slag fluidisation chlorination, carbide slag described in step a is TiC contents 11~15%, oxidation
Silicone content 25~29%, calcium oxide content 24~28%, content of magnesia 7~10%, alumina content 12~14%, carbon content
7~9%, other account for 1~2% carbide slag.
Wherein, in above-mentioned carbide slag fluidisation chlorination, carbide slag particle diameter described in step a is 80~800 mesh, preferably
120~400 mesh.When granularity is excessive, it is not easy to fluidize, chlorination effect is good；During undersized, reactor is easily blown, is caused
Titanium loses.
Wherein, in above-mentioned carbide slag fluidisation chlorination, the draw ratio of fluidized bed chlorination section described in step a is 20~
30:1。
Fluid bed of the present invention, the preferably upward fast fluidized bed of gas-solid cocurrent, can effectively be kept away using fluid bed
Exempting from carburizing reagent liberated heat makes local temperature in chlorination furnace higher so that and calcium oxide and magnesia reach chlorination temperature, from
And cohere defluidization problem when avoiding chlorination.
Wherein, in above-mentioned carbide slag fluidisation chlorination, the purity of chlorine gas feeding being passed through described in step a is 60~80%, is led to
The flow velocity for entering chlorine is 2~6m/s.In theory, it is the higher the better to be passed through the purity of chlorine, but considers for financial cost, above-mentioned carbon
In slugging fluidisation chlorination, purity of chlorine gas feeding is 60~80%.In order that chlorination reaction is more complete, the flow velocity of chlorine is passed through
For 2~6m/s, flow velocity is too fast, and carbide slag reaction is incomplete, and titanium tetrachloride yield is low, and flow velocity is excessively slow, and production efficiency is low, increase
Production cost and human cost.
Wherein, in above-mentioned carbide slag fluidisation chlorination, chlorination reaction temperature described in step a is 400~650 DEG C, chlorine
The change reaction time is 5~20min.
Wherein, in above-mentioned carbide slag fluidisation chlorination, lessivation is described in step b：Gas temperature by 450~
430 DEG C drop to 0~-5 DEG C by three-level elution.
Wherein, in order to save production cost, in above-mentioned carbide slag fluidisation chlorination, chlorine after being eluted in step b and
Recycled in fluid bed described in the equal return to step a of titanium tetrachloride.
In the method for the invention, carbonization solid impurity particle is added in fluid bed, in by process of air delivery, due to air-flow
Speed is fast, and the time mutually collided and contacted between particle is shorter, is advantageous to avoid particle from bonding agglomerate；Titanium carbide under high gas velocity
The exposed area in reaction zone is big, is advantageous to improve the chlorination rate of titanium carbide.The present invention can also be by chlorine superfluous in tail gas
Recycling is carried out, has effectively saved production cost.
Explanation is further explained to the embodiment of the present invention below by embodiment, but does not indicate that and sends out this
Bright protection domain is limited in described in embodiment in scope.
Carbide slag described in embodiment, which forms, is：By weight percentage, TiC contents 11~15%, silica content
25~29%, calcium oxide content 24~28%, content of magnesia 7~10%, alumina content 12~14%, carbon content 7~
9%, other account for 1~2% carbide slag.
Embodiment 1 carries out fluidisation chlorination with the inventive method to carbide slag
It is 20 that the carbide slag of 80~800 mesh particle diameters is sent into draw ratio:In 1 fast fluidized bed, with chlorine under fluidisation
Reacted, controlling reaction temperature is 650 DEG C.
Using above-mentioned carbide slag fast fluidization chloridization process, the quick chlorination reaction of carbide slag can be realized, it is whole to be pyrolyzed
Process control quickly takes unnecessary heat out of while the quick chlorination of completion titanium carbide in 10min, will not in chlorination furnace
Localized hyperthermia is produced, is produced without the material for causing to bond the generation of defluidization phenomenon.And fluidizing velocity is fast, the exposed of titanium carbide is increased
Area, its utilization rate is improved, for utilization rate up to more than 90%, the rate of recovery of chlorine is 80%.
Embodiment 2 carries out fluidisation chlorination with the inventive method to carbide slag
It is 20 that the carbide slag of 80~800 mesh particle diameters is sent into draw ratio:In 1 fast fluidized bed, with chlorine under fluidisation
Reacted, it is 650 DEG C to control furnace.
Using above-mentioned carbide slag fast fluidization chloridization process, the quick chlorination reaction of carbide slag can be realized, it is whole to be pyrolyzed
Process control quickly takes unnecessary heat out of while the quick chlorination of completion titanium carbide in 5min, will not in chlorination furnace
Localized hyperthermia is produced, is produced without the material for causing to bond the generation of defluidization phenomenon.And fluidizing velocity is fast, the exposed of titanium carbide is increased
Area, its utilization rate is improved, for utilization rate up to 85%, the rate of recovery of chlorine is 76%.
Embodiment 3 carries out fluidisation chlorination with the inventive method to carbide slag
It is 20 that the carbide slag of 80~800 mesh particle diameters is sent into draw ratio:In 1 fast fluidized bed, with chlorine under fluidisation
Reacted, it is 400 DEG C to control furnace.
Using above-mentioned carbide slag fast fluidization chloridization process, the quick chlorination reaction of carbide slag can be realized, it is whole to be pyrolyzed
Process control quickly takes unnecessary heat out of while the quick chlorination of completion titanium carbide in 5min, will not in chlorination furnace
Localized hyperthermia is produced, is produced without the material for causing to bond the generation of defluidization phenomenon.And fluidizing velocity is fast, the exposed of titanium carbide is increased
Area, its utilization rate is improved, for utilization rate up to 70%, the rate of recovery of chlorine is 70%.
Claims (9)
1. carbide slag fluidizes chlorination, it is characterised in that comprises the following steps：
A, carbonization solid impurity particle being put into fluid bed, is passed through chlorine and carries out chlorination reaction, chlorination reaction temperature is 400~650 DEG C,
The chlorination reaction time is 1~10min；
B, by the mixture obtained by step a after titanium tetrachloride elution circuit elutes and cools down, isolated chlorine and liquid
Titanium tetrachloride.
2. carbide slag according to claim 1 fluidizes chlorination, it is characterised in that：Carbide slag described in step a is TiC
Content 11~15%, silica content 25~29%, calcium oxide content 24~28%, content of magnesia 7~10%, aluminum oxide contains
Amount 12~14%, carbon content 7~9%, surplus are the carbide slag of impurity.
3. carbide slag according to claim 1 or 2 fluidizes chlorination, it is characterised in that：Be carbonized slag particle described in step a
Footpath is 80~800 mesh.
4. carbide slag according to claim 3 fluidizes chlorination, it is characterised in that：Carbide slag particle diameter described in step a
For 120~400 mesh.
5. carbide slag according to claim 3 fluidizes chlorination, it is characterised in that：Fluidized bed chlorination described in step a
The draw ratio of section is 20~30:1.
6. carbide slag according to claim 1 fluidizes chlorination, it is characterised in that：The flow velocity of chlorine is passed through in step a
For 2~6m/s.
7. carbide slag according to claim 1 fluidizes chlorination, it is characterised in that：The chlorine being passed through described in step a
Purity is 60~80%.
8. carbide slag according to claim 1 fluidizes chlorination, it is characterised in that：Lessivation is described in step b：
Gas temperature drops to 0~-5 DEG C by 450~430 DEG C by three-level elution, titanium tetrachloride yield >=98%.
9. carbide slag according to claim 1 fluidizes chlorination, it is characterised in that：Chlorine and tetrachloro described in step b
Change and recycled in fluid bed described in the equal return to step a of titanium.
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| CN201711014560.2A CN107601555A (en) | 2017-10-26 | 2017-10-26 | Carbide slag fluidizes chlorination |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109019601A (en) * | 2018-08-24 | 2018-12-18 | 攀钢集团攀枝花钢铁研究院有限公司 | The method for preparing carbide slag using sulfate process titanium dioxide acid hydrolysis residue |
| CN110372033A (en) * | 2019-08-19 | 2019-10-25 | 中国恩菲工程技术有限公司 | Titanium dioxide synthesis system |
| CN111663053A (en) * | 2020-06-29 | 2020-09-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Recycling method of titanium extraction tailings |
| CN115351053A (en) * | 2022-09-23 | 2022-11-18 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for treating chlorination tailings |
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| CN1454849A (en) * | 2002-04-30 | 2003-11-12 | 中国科学院过程工程研究所 | Apparatus and method of preparing titanium tetrachloride for chlorination of titanium-containing mineral |
| CN103028309A (en) * | 2012-12-26 | 2013-04-10 | 遵宝钛业有限公司 | Absorption method of chlorinated tail gas |
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| CN103028309A (en) * | 2012-12-26 | 2013-04-10 | 遵宝钛业有限公司 | Absorption method of chlorinated tail gas |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109019601A (en) * | 2018-08-24 | 2018-12-18 | 攀钢集团攀枝花钢铁研究院有限公司 | The method for preparing carbide slag using sulfate process titanium dioxide acid hydrolysis residue |
| CN110372033A (en) * | 2019-08-19 | 2019-10-25 | 中国恩菲工程技术有限公司 | Titanium dioxide synthesis system |
| CN111663053A (en) * | 2020-06-29 | 2020-09-15 | 攀钢集团攀枝花钢铁研究院有限公司 | Recycling method of titanium extraction tailings |
| CN115351053A (en) * | 2022-09-23 | 2022-11-18 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for treating chlorination tailings |
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Application publication date: 20180119 |