CN115351053B - Treatment method of chlorination tailings - Google Patents
Treatment method of chlorination tailings Download PDFInfo
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- CN115351053B CN115351053B CN202211162110.9A CN202211162110A CN115351053B CN 115351053 B CN115351053 B CN 115351053B CN 202211162110 A CN202211162110 A CN 202211162110A CN 115351053 B CN115351053 B CN 115351053B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/40—Destroying solid waste or transforming solid waste into something useful or harmless involving thermal treatment, e.g. evaporation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/70—Chemical treatment, e.g. pH adjustment or oxidation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B5/00—Operations not covered by a single other subclass or by a single other group in this subclass
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention belongs to the field of chloridizing metallurgy, and particularly relates to a treatment method of chloridizing tailings, which comprises the following steps: charging the titanium extraction chlorinated tailings mixed with a portion of the incompletely reacted chlorine gas into a fluidization apparatus; when the temperature is greater than or equal to a preset temperature, uniformly adding a dechlorinating agent into the fluidization equipment to perform dechlorination reaction; detecting whether the tail gas of the dechlorination reaction contains gas generated by combining cations and chloride ions in the dechlorination agent; and stopping the dechlorination reaction in response to the absence of gas in the tail gas generated by combination of cations in the dechlorinating agent and chloride ions. The invention utilizes the self temperature (500-550 ℃) of the titanium extraction tailings to carry out dechlorination reaction with FeO powder in a fluidized bed, does not need an external heat source, and can complete the dechlorination reaction by utilizing the self temperature of the titanium extraction tailings; the dechlorination process is short, the dechlorination reaction realizes the dechlorination treatment of chlorine and chlorine-containing compounds in one step, and provides a new idea for further comprehensive treatment of the titanium extraction tailings.
Description
Technical Field
The invention belongs to the field of chloridizing metallurgy, and particularly relates to a treatment method of chloridized tailings.
Background
The titanium-containing blast furnace slag is waste slag generated after vanadium titanomagnetite is ironed by a blast furnace, wherein the titanium content is up to 15-30%, how to extract the valuable titanium element is always a difficult problem, the most promising titanium extraction process route at present is a high-temperature carbonization technology and a low-temperature chlorination technology, the high-temperature carbonization technology converts TiO2 in the titanium-containing blast furnace slag into TiC, and the low-temperature chlorination technology converts TiC into TiCl 4 . The titanium extraction route has the advantages of short process flow, large processing capacity, high recovery rate of titanium resources and the like, and meanwhile, the titanium extraction chlorination tailings generated by the low-temperature chlorination technology in the process route contain a large amount of chlorine-containing compounds (MgCl) 2 ) And incompletely reacted chlorine gas, tiC, and the like. Due to the slag inThe tailings cannot be applied on a large scale due to the fact that a large amount of chlorine elements are contained.
Based on the above problems, the efficient dechlorination technology of the chlorinated tailings is particularly important, and there is room for improvement in the prior art.
Disclosure of Invention
This application summarizes aspects of the embodiments and should not be used to limit the claims. Other embodiments may be envisaged in light of the techniques described herein, as will be apparent to those skilled in the art upon studying the following drawings and detailed description, and are intended to be included within the scope of the present application.
Aiming at the problems existing in the prior art, the invention utilizes the self temperature (500-550 ℃) of the titanium extraction and chlorination tailings to perform dechlorination reaction with FeO powder in a fluidized bed, thereby realizing the deep dechlorination of the chlorination tailings.
Specifically, the invention provides a treatment method of chlorinated tailings, which comprises the following steps:
charging the titanium extraction chlorinated tailings mixed with a portion of the incompletely reacted chlorine gas into a fluidization apparatus;
when the temperature is greater than or equal to a preset temperature, uniformly adding a dechlorinating agent into the fluidization equipment to perform dechlorination reaction;
detecting whether the tail gas of the dechlorination reaction contains gas generated by combining cations and chloride ions in the dechlorination agent; and
the dechlorination reaction is stopped in response to the absence of gas in the tail gas generated by the combination of cations in the dechlorinating agent and chloride ions.
In an embodiment of the invention, the processing method further comprises the steps of:
detecting whether the titanium extraction chlorination tailings are fluidized into a fluidization state; and
detecting whether the temperature is greater than or equal to the predetermined temperature in response to fluidization of the titanium-extracting chlorinated tailings into a fluidized state.
In an embodiment of the invention, the predetermined temperature is 450 °.
In the embodiment of the invention, the addition amount of the dechlorinating agent is 10-15% of the mass of the titanium extraction and chlorination tailings.
In an embodiment of the invention, the dechlorinating agent is FeO powder.
In an embodiment of the invention, the dechlorination reaction comprises: extracting MgCl from titanium chloride tailings by the following reaction formulas one and two at 300-500 DEG C 2 Conversion of incompletely reacted chlorine and TiC to MgO and TiO 2 Whereas FeO powder is converted into FeCl 3 And (3) discharging gas:
Cl 2 +2FeO+2MgCl 2 ＝2FeCl 3 +2MgO reaction type I
9Cl 2 +6FeO+2TiC＝6FeCl 3 +2TiO 2 +2co equation two.
In the embodiment of the invention, the titanium extraction and chlorination tailings comprise 1 to 4 percent of MgCl 2 。
In the embodiment of the invention, whether the tail gas of the dechlorination reaction contains gas generated by combining cations and chloride ions in the dechlorination agent is detected; and stopping the dechlorination reaction in response to the absence of gas in the tail gas generated by combination of cations in the dechlorinating agent and chloride ions, comprising:
detecting whether the tail gas of the dechlorination reaction contains FeCl 3 The method comprises the steps of carrying out a first treatment on the surface of the And
in response to absence of FeCl in the tail gas 3 While stopping the dechlorination reaction.
In an embodiment of the invention, the temperature of the titanium extraction chlorination tailings loaded into the fluidization equipment is 500-550 ℃ per se, and no additional heat source is needed for the dechlorination reaction.
In an embodiment of the invention, the fluidization device is a bubbling fluidized bed.
The invention utilizes the self temperature (500-550 ℃) of the titanium extraction tailings to carry out dechlorination reaction with FeO powder in a fluidized bed, does not need an external heat source, and can complete the dechlorination reaction by utilizing the self temperature of the titanium extraction tailings; the dechlorination process is short, the dechlorination reaction realizes the dechlorination treatment of chlorine and chlorine-containing compounds in one step, and provides a new idea for further comprehensive treatment of the titanium extraction tailings.
These and other aspects, objects, and features of the present disclosure will be understood and appreciated by those skilled in the art upon studying the following specification, claims, and appended drawings.
Drawings
For a more complete understanding of the embodiments of the present application, reference should be made to the embodiments illustrated in greater detail in the accompanying drawings and described below by way of example, wherein:
fig. 1 shows a flow chart of a method of treating chlorinated tailings according to an embodiment of the invention.
Detailed Description
Embodiments of the present disclosure are described below. However, it is to be understood that the disclosed embodiments are merely examples and that other embodiments may take various alternative forms. The figures are not necessarily to scale; some functions may be exaggerated or minimized to show details of particular components. Therefore, specific structural and functional details disclosed herein are not to be interpreted as limiting, but merely as a representative basis for teaching one skilled in the art to variously employ the present application. As will be appreciated by those skilled in the art, the various features illustrated and described with reference to any one drawing may be combined with features illustrated in one or more other drawings to produce embodiments that are not explicitly illustrated or described. The combination of features shown provides representative embodiments for typical applications. However, various combinations and modifications of the features consistent with the teachings of the present disclosure may be desired for certain specific applications or implementations.
Moreover, in this document, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. The terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
One or more embodiments of the present application will be described below with reference to the accompanying drawings. The flow diagrams illustrate the processes performed by systems according to the present application, it being understood that the flow diagrams need not be performed in order, that one or more steps may be omitted, that one or more steps may be added, and that one or more steps may be performed in order or in reverse order, or even simultaneously in some embodiments.
The invention provides a treatment method of chlorinated tailings, which aims to solve the existing technical problems of low-temperature chlorination technology of titanium-containing blast furnace slag. The method takes chloridized tailings as raw materials, mgCl 2 FeO powder with the content of 1-4% is dechlorinating agent, the fluidized bed is fluidization equipment, and Cl is reacted at 300-500 DEG C 2 +2FeO+2MgCl 2 ＝2FeCl 3 +2MgO、9Cl 2 +6FeO+2TiC＝6FeCl 3 +2TiO 2 +2CO will chlorinate MgCl in tailings 2 Incompletely reacted Cl 2 And TiC is converted into harmless MgO and TiO 2 Whereas FeO powder is converted into FeCl 3 And (5) discharging the gas. The slag can realize complete dechlorination, and can be used as a general building material.
Specifically, according to the present invention, there is provided a treatment method of chlorinated tailings, as shown in fig. 1, comprising the steps of:
s101, filling titanium extraction and chlorination tailings mixed with a part of incompletely reacted chlorine into fluidization equipment;
s103, uniformly adding a dechlorinating agent into the fluidization equipment to perform dechlorination reaction when the temperature is more than or equal to a preset temperature;
s105, detecting whether the tail gas of the dechlorination reaction contains gas generated by combining cations and chloride ions in the dechlorination agent; and
s107. stopping the dechlorination reaction in response to the absence of gas in the tail gas generated by combination of cations in the dechlorinating agent and chloride ions.
In step S101, a part of chlorine gas which is not fully reacted is directly mixed during slag removal of the titanium extraction and chlorination tailings, and the chlorine gas is heated and filled into dechlorination fluidization equipment, wherein the temperature of the titanium extraction tailings is about 500-600 ℃. In one embodiment, the desulfurization fluidization device may be a bubbling fluidized bed. The titanium extraction and chlorination tailings can be directly derived from titanium-containing blast furnace slag after high-temperature carbonization.
In step S103, the treatment method may further include detecting whether the titanium extraction chlorinated tailings are fluidized into a fluidized state; and detecting whether the temperature is greater than or equal to the predetermined temperature in response to fluidization of the titanium-extracted chlorinated tailings into a fluidized state.
In one embodiment, the dechlorinating agent can be FeO powder, when the titanium extraction tailings are fluidized into a fluidized state, when the temperature is detected to be not lower than 450 ℃ by a thermocouple, the FeO powder is added into the dechlorinating fluidized bed at a constant speed, the addition amount is 10-15% of the mass of the titanium extraction tailings, and dechlorination reaction immediately occurs.
In step 105, it may be detected in real time or at predetermined intervals (e.g., 5-20 minutes) whether the tail gas of the dechlorination reaction contains a gas generated by combining cations in the dechlorinating agent with chloride ions. In the case that the dechlorinating agent is FeO powder, whether FeCl is contained in the tail gas of the dechlorination reaction can be detected in real time or at intervals of a predetermined time 3 。
In step 107, if no gas is detected in the tail gas that is generated by the combination of cations and chloride ions in the dechlorination agent, indicating that the dechlorination reaction is substantially complete, the dechlorination reaction may be stopped. In one embodiment, in response to detecting that the tail gas does not include FeCl 3 The dechlorination reaction is stopped.
In an embodiment of the invention, the dechlorination reaction comprises: extracting MgCl from titanium chloride tailings by the following reaction formulas one and two at 300-500 DEG C 2 Conversion of incompletely reacted chlorine and TiC to MgO and TiO 2 Whereas FeO powder is converted into FeCl 3 And (3) discharging gas:
Cl 2 +2FeO+2MgCl 2 ＝2FeCl 3 +2MgO reaction type I
9Cl 2 +6FeO+2TiC＝6FeCl 3 +2TiO 2 +2CO reactionAnd formula II.
The CO produced may be collected by means commonly used in the art and will not be described in detail herein.
In the embodiment of the invention, the self temperature of the titanium extraction and chlorination tailings filled in the fluidization equipment is 500-550 ℃, so that no additional heat source is needed in the dechlorination reaction.
The invention is further illustrated by the following specific examples, it being understood that the following examples are illustrative of the invention and are not intended to limit the scope of the invention.
In particular to a preferred embodiment, the method adopts
200g of titanium extraction tailings of a fluidized bed with a boiling bed, wherein MgCl 2 The content is 8g, feO powder 20g. Firstly, 200g of titanium extraction tailings are hot-charged into +.>
The thermocouple shows temperature of 550 ℃ in the boiling fluidized bed, then 20g of FeO powder is added at constant speed, dechlorination reaction is started in the fluidized bed, and FeCl overflows 3 The reaction was stopped after about 15min with gas. Sampling analysis of dechlorinated titanium tailings, mgCl thereof 2 The content is less than or equal to 0.5 percent.
After the invention is implemented, the beneficial effects are as follows: the dechlorination reaction can be completed by utilizing the self temperature of the titanium extraction chlorination tailings without an external heat source; the dechlorination process is short, the dechlorination reaction realizes the dechlorination treatment of chlorine and chlorine-containing compounds in one step, and provides a new idea for further comprehensive treatment of the titanium extraction tailings.
This application is intended to cover any adaptations or variations of the disclosed techniques and various embodiments and is not intended to limit the true scope and spirit of the disclosed techniques and embodiments. Moreover, the foregoing description is not intended to be exhaustive or to limit the scope of the invention to the precise form disclosed. Modifications and variations are possible in light of the above teachings. The embodiments were chosen and described to provide the best illustration of the principles of the technology and its practical application, and to enable one of ordinary skill in the art to utilize the disclosed technology in various modifications as are suited to the particular use contemplated. Accordingly, various changes and modifications to the above-described embodiments are intended to be included within the scope of the present disclosure without materially departing from the spirit and principles of the techniques described herein.
Claims (8)
1. The treatment method of the chlorination tailings is characterized by comprising the following steps:
charging the titanium extraction chlorinated tailings mixed with a portion of the incompletely reacted chlorine gas into a fluidization apparatus;
when the temperature is greater than or equal to a preset temperature, uniformly adding a dechlorinating agent into the fluidization equipment to perform dechlorination reaction;
detecting whether the tail gas of the dechlorination reaction contains gas generated by combining cations and chloride ions in the dechlorination agent; and
stopping the dechlorination reaction in response to the absence of gas in the tail gas generated by combination of cations in the dechlorinating agent and chloride ions,
wherein the dechlorinating agent is FeO powder, and the dechlorinating reaction comprises: extracting MgCl from titanium chloride tailings by the following reaction formulas one and two at 300-500 DEG C 2 Conversion of incompletely reacted chlorine and TiC to MgO and TiO 2 Whereas FeO powder is converted into FeCl 3 And (3) discharging gas:
Cl 2 +2FeO+2MgCl 2 ＝2FeCl 3 +2MgO reaction type I
9Cl 2 +6FeO+2TiC＝6FeCl 3 +2TiO 2 +2co equation two.
2. The method of treating chlorinated tailings of claim 1, further comprising the steps of:
detecting whether the titanium extraction chlorination tailings are fluidized into a fluidization state; and
detecting whether the temperature is greater than or equal to the predetermined temperature in response to fluidization of the titanium-extracting chlorinated tailings into a fluidized state.
3. The method of treating chlorinated tailings of claim 2, wherein the predetermined temperature is 450 °.
4. The method for treating chlorinated tailings according to claim 1, wherein the dechlorinating agent is added in an amount of 10-15% of the mass of the titanium-extracted chlorinated tailings.
5. The method for treating chlorinated tailings according to claim 1, wherein the titanium extraction chlorinated tailings comprise 1% -4% MgCl 2 。
6. The method for treating chlorinated tailings according to claim 1, wherein the tail gas of the dechlorination reaction is detected to contain a gas generated by combining cations and chloride ions in the dechlorination agent; and stopping the dechlorination reaction in response to the absence of gas in the tail gas generated by combination of cations in the dechlorinating agent and chloride ions, comprising:
detecting whether the tail gas of the dechlorination reaction contains FeCl 3 The method comprises the steps of carrying out a first treatment on the surface of the And
in response to absence of FeCl in the tail gas 3 While stopping the dechlorination reaction.
7. The method for treating chlorinated tailings according to claim 1, wherein the self temperature of the titanium extracted chlorinated tailings charged into the fluidization apparatus is 500 ℃ to 550 ℃, and the dechlorination reaction is performed without additional heat source.
8. The method of treating chlorinated tailings of claim 1, wherein the fluidization apparatus is a bubbling fluidized bed.
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