CN105984894B - Method and system for preparing refined titanium tetrachloride - Google Patents

Method and system for preparing refined titanium tetrachloride Download PDF

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Publication number
CN105984894B
CN105984894B CN201510053934.6A CN201510053934A CN105984894B CN 105984894 B CN105984894 B CN 105984894B CN 201510053934 A CN201510053934 A CN 201510053934A CN 105984894 B CN105984894 B CN 105984894B
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titanic chloride
titanium tetrachloride
crude
crude titanic
chloride
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CN105984894A (en
Inventor
刘建良
李增光
龙翔
钱春花
赵泽权
杨易邦
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Gansu Detongguo Titanium Metal Co ltd
Yunnan Guoti Metal Co ltd
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Yunnan Metallurgical Xinli Titanium Industry Co ltd
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Abstract

The invention provides a method and a system for preparing refined titanium tetrachloride, wherein the method for preparing the refined titanium tetrachloride comprises the following steps: adding high titanium slag and petroleum coke into a chlorination furnace, and carrying out chlorination reaction with chlorine introduced into the chlorination furnace in a boiling state so as to obtain crude titanium tetrachloride steam; condensing the crude titanium tetrachloride vapor to obtain crude titanium tetrachloride; mixing the crude titanium tetrachloride with an organic reagent through a pipeline mixer and conveying the mixture into evaporation equipment; and subjecting the crude titanium tetrachloride to an evaporation treatment in an evaporation apparatus to obtain refined titanium tetrachloride. The method can be used for effectively preparing the refined titanium tetrachloride with higher purity.

Description

Prepare the method and system of refined titanic chloride
Technical field
The invention belongs to field of titanium dioxide production, specifically, the present invention relates to the method for preparing refined titanic chloride and is System.
Background technology
Titanium dioxide is prepared at present and prepares titanium tetrachloride first, recycles titanium tetrachloride to occur with oxygen in oxidation furnace soon TiO is obtained after fast high-temperature oxydation reaction2The Titanium Dioxide Produced by Chloride Procedure of high quality is made in base-material, base-material after after process processing.So And it is TiO that the committed step for often influenceing titanium dioxide finished product quality at present, which is not,2The purification of base-material, but producing four chlorinations Due to containing impurity in supplementary material during titanium, caused by produce impurity content in obtained titanium tetrachloride high, and then lead Cause finally be prepared using the titanium tetrachloride finished product titanium dioxide it is second-rate.Therefore, it is relevant at present to prepare high-purity The method of titanium tetrachloride be further improved.
The content of the invention
It is contemplated that at least solves one of technical problem in correlation technique to a certain extent.Therefore, the present invention One purpose is to propose a kind of method and system that the higher refined titanic chloride of purity can effectively be prepared.
According to an aspect of the present invention, the present invention proposes a kind of method for preparing refined titanic chloride, and this method includes:
High titanium slag and petroleum coke are added in chlorination furnace and the chlorine with being passed through in the chlorination furnace is under fluidized states Generation chlorination reaction, to obtain crude titanic chloride steam;
The crude titanic chloride steam is subjected to condensation process, to obtain crude titanic chloride;
The crude titanic chloride is mixed and is delivered in evaporation equipment by pipe-line mixer with organic reagent;And
The crude titanic chloride is set to be evaporated processing in evaporation equipment, to obtain refined titanic chloride.
Thus, using the method for preparing refined titanic chloride of the above embodiment of the present invention, by crude titanic chloride and organic examination Agent can significantly improve the two degree of mixedness by pipe-line mixer mixing, and crude titanic chloride is removed it is possible thereby to further improve The efficiency and effect of the impurity such as middle iron, vanadium, the higher refined titanic chloride of purity is finally prepared.
The method for preparing refined titanic chloride according to embodiments of the present invention further comprises:
The titanium tetrachloride obtained by the evaporation process is delivered in multiple titanium tetrachloride storage tanks stage by stage;
The titanium tetrachloride in the multiple titanium tetrachloride storage tank is detected respectively, to obtain the qualified essence of purity Titanium tetrachloride and/or the underproof titanium tetrachloride of purity;
The underproof titanium tetrachloride of purity is returned and is mixed with organic reagent by pipe-line mixer and carries out the evaporation Processing.
According to some embodiments of the present invention, the high titanium slag is rutile, and the organic reagent is mineral oil.
According to some embodiments of the present invention, the mixed weight ratio of the crude titanic chloride and organic reagent is 100: 0.05-0.5。
According to some embodiments of the present invention, in the pipe-line mixer, the crude titanic chloride mixes with organic reagent The flow velocity of thing is 20t/h.
According to some embodiments of the present invention, content of vanadium is 180ppm in the crude titanic chloride, the refined titanic chloride Middle content of vanadium is no more than 3ppm.
According to the second aspect of the invention, the present invention proposes a kind of system for preparing refined titanic chloride, and the system includes:
Boiling chloridizing furnace, the boiling chloridizing furnace have high titanium slag entrance, petroleum coke entrance, chlorine inlet and thick four chlorination Titanium steam (vapor) outlet, the boiling chloridizing furnace are suitable to high titanium slag and petroleum coke and thick four chlorination are prepared with chlorine generation chlorination reaction Titanium steam;
There is crude titanic chloride steam inlet and crude titanic chloride to export for condensing unit, the condensing unit, and described thick four Titanium chloride steam inlet is connected with the crude titanic chloride steam (vapor) outlet;
Pipe-line mixer, the pipe-line mixer have crude titanic chloride entrance, organic reagent entrance and mixture outlet, The crude titanic chloride entrance is connected with crude titanic chloride outlet, and the pipe-line mixer is suitable to crude titanic chloride with having Machine reagent is mixed and conveyed;And
Evaporation equipment, the evaporation equipment are connected with the mixture outlet, and are evaporated processing suitable for mixture, with Just refined titanic chloride is obtained.
Thus, using the method for preparing refined titanic chloride of the above embodiment of the present invention, by crude titanic chloride and organic examination Agent can significantly improve the two degree of mixedness by pipe-line mixer mixing, and crude titanic chloride is removed it is possible thereby to further improve The efficiency and effect of the impurity such as middle iron, vanadium, the higher refined titanic chloride of purity is finally prepared.
The system for preparing refined titanic chloride according to embodiments of the present invention further comprises:
Crude titanic chloride storage tank, the crude titanic chloride storage tank are located at the condensing unit and the pipe-line mixer Between.
The system for preparing refined titanic chloride according to embodiments of the present invention further comprises:
Multiple titanium tetrachloride storage tanks, the multiple titanium tetrachloride storage tank are connected with the evaporation equipment respectively,
Optionally, at least one in the multiple titanium tetrachloride storage tank is connected with the crude titanic chloride storage tank.
According to some embodiments of the present invention, the multiple titanium tetrachloride storage tank is two.
Brief description of the drawings
Fig. 1 is the flow chart of the method according to an embodiment of the invention for preparing refined titanic chloride.
Fig. 2 is the structure chart of the system according to an embodiment of the invention for preparing refined titanic chloride.
Embodiment
Embodiments of the invention are described below in detail, the example of the embodiment is shown in the drawings, wherein from beginning to end Same or similar label represents same or similar element or the element with same or like function.Below with reference to attached The embodiment of figure description is exemplary, it is intended to for explaining the present invention, and is not considered as limiting the invention.
The method for preparing refined titanic chloride of the embodiment of the present invention is described in detail below with reference to Fig. 1, according to of the invention specific The method for preparing refined titanic chloride of embodiment includes:
High titanium slag and petroleum coke are added in chlorination furnace and the chlorine with being passed through in the chlorination furnace is under fluidized states Generation chlorination reaction, to obtain crude titanic chloride steam;
The crude titanic chloride steam is subjected to condensation process, to obtain crude titanic chloride;
The crude titanic chloride is mixed and is delivered in evaporation equipment by pipe-line mixer with organic reagent;And
The crude titanic chloride is set to be evaporated processing in evaporation equipment, to obtain refined titanic chloride.
Thus, using the method for preparing refined titanic chloride of the above embodiment of the present invention, by crude titanic chloride and organic examination Agent can significantly improve the two degree of mixedness by pipe-line mixer mixing, and crude titanic chloride is removed it is possible thereby to further improve The efficiency and effect of the impurity such as middle iron, vanadium, the higher refined titanic chloride of purity is finally prepared.
According to a particular embodiment of the invention, the method for preparing refined titanic chloride of above-described embodiment can also be wrapped further Include:The titanium tetrachloride obtained by the evaporation process is delivered in multiple titanium tetrachloride storage tanks stage by stage;Respectively to institute The titanium tetrachloride stated in multiple titanium tetrachloride storage tanks is detected, to obtain the qualified refined titanic chloride of purity and/or purity Underproof titanium tetrachloride;The underproof titanium tetrachloride of purity is returned and mixes and carries out by pipe-line mixer with organic reagent The evaporation process.It is possible thereby to the purity of the titanium tetrachloride after purification is checked on, by the underproof titanium tetrachloride of purity Return carries out purification processes again, thus avoids by mistake being used to the unqualified titanium tetrachloride of purity prepare titanium dioxide, influences finished product Quality.
According to a particular embodiment of the invention, the content of vanadium in the crude titanic chloride being prepared first in chlorination furnace is 180ppm, and further crude titanic chloride is mixed with organic reagent removal of impurities processing is carried out to it.Due to crude titanic chloride with Organic reagent is respectively aqueous phase and oil phase, therefore the two well mixed difficulty is bigger, the preparation essence of the embodiment of the present invention The method of titanium tetrachloride highly hits the two by using pipe-line mixer during conveying realizes the effectively mixed of the two Close, and it is higher using both this method degree of mixedness, and then effectively can remove essence using finely dispersed organic reagent The impurity contained in titanium tetrachloride, and then refined titanic chloride purity is improved, finally to improve the purity of finished product titanium dioxide.Together Shi Caiyong pipe-line mixers are mixed crude titanic chloride with organic reagent, and thick tetrachloro can also be completed during mixing Change titanium to the conveying to evaporation equipment, and then raising prepares the efficiency of refined titanic chloride.
According to a particular embodiment of the invention, by using the method for preparing refined titanic chloride of the above embodiment of the present invention The crude titanic chloride that can be 180ppm by content of vanadium purifies to purity as the refined titanic chloride no more than 3ppm.Thus utilizing should Refined titanic chloride prepares titanium dioxide, can notable titanium dioxide quality.
According to a particular embodiment of the invention, the above-mentioned raw material high titanium slag for being used to prepare crude titanic chloride can be golden red Stone.Preferably, the organic reagent for removal of impurities can be mineral oil, and thus crude titanic chloride is carried using the organic reagent The pure purity that can significantly improve refined titanic chloride, and then improve the purity that titanium dioxide finished product is prepared using refined titanic chloride.
According to a particular embodiment of the invention, can by crude titanic chloride and organic reagent in pipe-line mixer according to 100:0.05-0.5 weight ratio is mixed, and in other words, is added according to the 0.05-0.5 weight % of crude titanic chloride organic Reagent, it is possible thereby to significantly improve Blending Efficiency of Blending and impurity-eliminating effect.Inventors herein have recognized that impurity-eliminating effect not with it is organic The addition of reagent is directly proportional, when the addition of organic reagent is apparently higher than 0.5 weight %, crude titanic chloride and organic reagent To be divided into effect obvious, therefore, the difficulty for causing the two to mix is bigger, and impurity-eliminating effect reduces on the contrary.Therefore, by big Verification experimental verification is measured, 0.05-0.5 weight % organic reagents are added into crude titanic chloride can significantly improve the Blending Efficiency of Blending of the two And impurity-eliminating effect.According to the specific example of the present invention, content of vanadium can be prepared by using the above method and be not more than 3ppm Refined titanic chloride, and then can further improve using its preparation finished product titanium dioxide purity.
, can be by crude titanic chloride and organic reagent in pipe-line mixer according to the another specific embodiment of the present invention Mixture is mixed and conveyed with 20t/h flow velocity, it is possible thereby to further improve the degree of mixedness of the two.Invention human hair Existing, if flow velocity is excessively slow, the two shock in pipe-line mixer is inadequate, finally influences Blending Efficiency of Blending;If flow velocity is too fast, meeting Significantly shorten incorporation time, can equally influence final mixed effect.Therefore, can using the flow velocity of the above embodiment of the present invention To significantly improve the degree of mixedness of the two, and then the purity of refined titanic chloride is improved, its preparation is utilized further to improve The purity of finished product titanium dioxide.
According to the second aspect of the invention, the present invention proposes a kind of system for preparing refined titanic chloride.
The system for preparing refined titanic chloride of the specific embodiment of the invention is described in detail below with reference to Fig. 2, according to the present invention The system 100 for preparing refined titanic chloride of specific embodiment includes:Boiling chloridizing furnace 10, condensing unit 20, pipe-line mixer 30 With evaporation equipment 40.
Wherein, there is boiling chloridizing furnace high titanium slag entrance 11, petroleum coke entrance 12, chlorine inlet 13 and crude titanic chloride to steam Vapor outlet 14, boiling chloridizing furnace 10 are suitable to high titanium slag and petroleum coke and crude titanic chloride steaming are prepared with chlorine generation chlorination reaction Vapour;Condensing unit 20 has crude titanic chloride steam inlet 21 and crude titanic chloride outlet 22, crude titanic chloride steam inlet 21 It is connected with crude titanic chloride steam (vapor) outlet 14;Pipe-line mixer 30 has crude titanic chloride entrance 31, the and of organic reagent entrance 32 Mixture outlet 33, crude titanic chloride entrance 31 are connected with crude titanic chloride outlet 22, and pipe-line mixer is suitable to thick four chlorination Titanium is mixed and conveyed with organic reagent;And evaporation equipment 40 is connected with mixture outlet 33, and carried out suitable for mixture Evaporation process, to obtain refined titanic chloride.
Thus, using the system for preparing refined titanic chloride of the above embodiment of the present invention, by crude titanic chloride and organic examination Agent can significantly improve the two degree of mixedness by pipe-line mixer mixing, and crude titanic chloride is removed it is possible thereby to further improve The efficiency and effect of the impurity such as middle iron, vanadium, the higher refined titanic chloride of purity is finally prepared.
Further comprised according to the system for preparing refined titanic chloride of the specific embodiment of the invention:Crude titanic chloride storage tank 50。
Crude titanic chloride storage tank 50 is located between condensing unit 20 and pipe-line mixer 30.It is possible thereby to ensure that pipeline mixes The continuous operation of clutch 30, predetermined conveying flow velocity is maintained, and then improve the degree of mixedness of crude titanic chloride and organic reagent, entered And improve the purity of the finished product titanium dioxide using its preparation.
Further comprised according to the system for preparing refined titanic chloride of the specific embodiment of the invention:Multiple titanium tetrachloride storages Tank 60, multiple titanium tetrachloride storage tanks are connected with the evaporation equipment respectively.It is possible thereby to by stages to being made in evaporation equipment Standby obtained titanium tetrachloride is stored.And the purity of the titanium tetrachloride in each titanium tetrachloride storage tank can be entered respectively Whether qualified row detection, analyze its purity.
According to a particular embodiment of the invention, at least one and crude titanic chloride in above-mentioned multiple titanium tetrachloride storage tanks Storage tank is connected.It is possible thereby to be checked on to the purity of the titanium tetrachloride after purification, the underproof titanium tetrachloride of purity is returned Return and carry out purification processes again, thus avoid by mistake being used to the unqualified titanium tetrachloride of purity prepare titanium dioxide, influence finished product Quality.
Preferably, as shown in Fig. 2 above-mentioned multiple titanium tetrachloride storage tanks are two.
In the present invention, unless otherwise clearly defined and limited, term " installation ", " connected ", " connection ", " fixation " etc. Term should be interpreted broadly, for example, it may be fixedly connected or be detachably connected, or integrally;Can be that machinery connects Connect or electrically connect;Can be joined directly together, can also be indirectly connected by intermediary, can be in two elements The connection in portion or the interaction relationship of two elements.For the ordinary skill in the art, can be according to specific feelings Condition understands the concrete meaning of above-mentioned term in the present invention.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show The description of example " or " some examples " etc. means specific features, structure, material or the spy for combining the embodiment or example description Point is contained at least one embodiment or example of the present invention.In this manual, to the schematic representation of above-mentioned term not Identical embodiment or example must be directed to.Moreover, specific features, structure, material or the feature of description can be any Combined in an appropriate manner in individual or multiple embodiments or example.In addition, in the case of not conflicting, the technology of this area Different embodiments or example and the feature of different embodiments or example described in this specification can be combined by personnel And combination.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment is example Property, it is impossible to limitation of the present invention is interpreted as, one of ordinary skill in the art within the scope of the invention can be to above-mentioned Embodiment is changed, changed, replacing and modification.

Claims (8)

  1. A kind of 1. method for preparing refined titanic chloride, it is characterised in that including:
    High titanium slag and petroleum coke are added in chlorination furnace and the chlorine with being passed through in the chlorination furnace occurs under fluidized state Chlorination reaction, to obtain crude titanic chloride steam;
    The crude titanic chloride steam is subjected to condensation process, to obtain crude titanic chloride;
    The crude titanic chloride is mixed and is delivered in evaporation equipment by pipe-line mixer with mineral oil;And
    The crude titanic chloride is set to be evaporated processing in evaporation equipment, to obtain refined titanic chloride,
    The mixed weight ratio of the crude titanic chloride and mineral oil is 100:0.05-0.5,
    Flow velocity of the mixture of the crude titanic chloride and the mineral oil in the pipe-line mixer is 20t/h.
  2. 2. the method according to claim 1 for preparing refined titanic chloride, it is characterised in that further comprise:
    The titanium tetrachloride obtained by the evaporation process is delivered in multiple titanium tetrachloride storage tanks stage by stage;
    The titanium tetrachloride in the multiple titanium tetrachloride storage tank is detected respectively, to obtain the qualified smart tetrachloro of purity Change titanium and/or the underproof titanium tetrachloride of purity;
    The underproof titanium tetrachloride of purity is returned and is mixed with mineral oil by pipe-line mixer and carries out the evaporation process.
  3. 3. the method according to claim 1 or 2 for preparing refined titanic chloride, it is characterised in that the high titanium slag is golden red Stone.
  4. 4. the method according to claim 1 for preparing refined titanic chloride, it is characterised in that vanadium contains in the crude titanic chloride It is no more than 3ppm to measure as 180ppm, the refined titanic chloride content of vanadium.
  5. A kind of 5. system for preparing refined titanic chloride, it is characterised in that including:
    There is high titanium slag entrance, petroleum coke entrance, chlorine inlet and crude titanic chloride to steam for boiling chloridizing furnace, the boiling chloridizing furnace Vapor outlet, the boiling chloridizing furnace are suitable to high titanium slag and petroleum coke and crude titanic chloride steaming are prepared with chlorine generation chlorination reaction Vapour;
    Condensing unit, the condensing unit have crude titanic chloride steam inlet and crude titanic chloride outlet, thick four chlorination Titanium steam inlet is connected with the crude titanic chloride steam (vapor) outlet;
    Pipe-line mixer, the pipe-line mixer has crude titanic chloride entrance, organic reagent entrance and mixture outlet, described Crude titanic chloride entrance is connected with crude titanic chloride outlet, and the pipe-line mixer is suitable to crude titanic chloride and mineral oil Mixed and conveyed;And
    Evaporation equipment, the evaporation equipment are connected with the mixture outlet, and are evaporated processing suitable for mixture, so as to To refined titanic chloride.
  6. 6. the system according to claim 5 for preparing refined titanic chloride, it is characterised in that further comprise:
    Crude titanic chloride storage tank, the crude titanic chloride storage tank be located at the condensing unit and the pipe-line mixer it Between.
  7. 7. the system according to claim 6 for preparing refined titanic chloride, it is characterised in that further comprise:
    Multiple titanium tetrachloride storage tanks, the multiple titanium tetrachloride storage tank are connected with the evaporation equipment respectively,
    At least one in the multiple titanium tetrachloride storage tank is connected with the crude titanic chloride storage tank.
  8. 8. the system according to claim 7 for preparing refined titanic chloride, it is characterised in that the multiple titanium tetrachloride storage Tank is two.
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CN109022827B (en) * 2018-07-04 2020-10-20 南京理工大学 Method for directly preparing TiAl alloy from titanium ore
CN109052463A (en) * 2018-10-30 2018-12-21 攀钢集团攀枝花钢铁研究院有限公司 A kind of purification of crude titanic chloride removes vanadium method

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CN103693684B (en) * 2013-12-09 2016-02-10 云南冶金新立钛业有限公司 Prepare the method and system of titanium dioxide
CN203668021U (en) * 2013-12-09 2014-06-25 云南新立有色金属有限公司 System for preparing titanium dioxide
CN103693685B (en) * 2013-12-09 2015-11-25 云南新立有色金属有限公司 Prepare the method for titanium dioxide
CN103896329B (en) * 2013-12-09 2016-06-01 云南冶金新立钛业有限公司 Prepare the system of titanium tetrachloride
CN103880074B (en) * 2013-12-09 2015-11-25 云南新立有色金属有限公司 Prepare the method for titanium dioxide
CN103896333B (en) * 2013-12-09 2015-11-25 云南新立有色金属有限公司 Prepare the method for titanium dioxide
CN103693687B (en) * 2013-12-09 2015-06-24 云南新立有色金属有限公司 Method and system for preparing titanium dioxide

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