CN115475696A - Method for recycling dust collection slag of fused salt chlorination furnace - Google Patents

Method for recycling dust collection slag of fused salt chlorination furnace Download PDF

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Publication number
CN115475696A
CN115475696A CN202211182521.4A CN202211182521A CN115475696A CN 115475696 A CN115475696 A CN 115475696A CN 202211182521 A CN202211182521 A CN 202211182521A CN 115475696 A CN115475696 A CN 115475696A
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China
Prior art keywords
filtrate
dust collection
chlorination furnace
tailings
collection slag
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Pending
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CN202211182521.4A
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Chinese (zh)
Inventor
李建军
业震宇
黄海广
陈建立
祝永红
杨德
张美杰
卢伟伟
侯廉杰
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Yunnan Guoti Metal Co ltd
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Yunnan Guoti Metal Co ltd
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Priority to CN202211182521.4A priority Critical patent/CN115475696A/en
Publication of CN115475696A publication Critical patent/CN115475696A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03BSEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B9/00General arrangement of separating plant, e.g. flow sheets
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention belongs to the technical field of recycling of waste and side materials in chemical production, and particularly relates to a method for recycling dust collection slag of a molten salt chlorination furnace, which comprises the following steps: dissolving titanium tetrachloride dust collection slag in a hydrochloric acid solution to obtain a sizing agent; separating concentrate and first tailings from the slurry through flotation; reselecting the concentrate through a table concentrator to obtain titanium concentrate, second tailings and second filtrate, and performing filter pressing on the first tailings to obtain first filtrate and coke-containing filter residue; and carrying out MVR treatment on the first filtrate and the second filtrate. The purpose is as follows: through reasonable improvement of the prior art, the titanium-rich material in the titanium tetrachloride dust-collecting slag is effectively recovered, the processing cost of the dust-collecting slag is reduced, valuable resources are recovered, and the process flow is shortened.

Description

Method for recycling dust collection slag of fused salt chlorination furnace
Technical Field
The invention belongs to the technical field of recycling of waste and side materials in chemical production, and particularly relates to a method for recycling dust collection slag of a molten salt chlorination furnace.
Background
At present, the production process of titanium tetrachloride mainly comprises a boiling chlorination method and a molten salt chlorination method, wherein the molten salt chlorination method is to react a solid titanium-containing material with gaseous chlorine in medium molten salt. The titanium tetrachloride is discharged out of the chlorination furnace in a steam form after being generated, crude titanium tetrachloride solution is obtained through subsequent condensation, dust collection slag is mainly formed by mixing small-particle titanium ore and coke in titanium tetrachloride steam, and the titanium tetrachloride steam is separated through a gravity dust collector to obtain the dust collection slag. The prior art directly sends the dust-collecting slag to a slag yard for treatment, thereby causing resource waste.
0.03t of dust collecting slag is generated when 1 ton of titanium tetrachloride is produced in the dust collecting slag in the gravity dust collecting procedure of the molten salt chlorination furnace. The dust-collecting slag has high coke content of high titanium slag and fine grains, the residual components are mainly NaCl, fe, nb and other substances, an effective treatment method for the titanium tetrachloride dust-collecting slag is lacked in the prior art, most enterprises adopt a method of landfill or accumulation after solidification to treat the titanium tetrachloride dust-collecting slag, and resource waste and environmental pollution are caused.
Therefore, a new recycling treatment process for the dust-collecting slag of the molten salt chlorination furnace is needed to be developed, waste recycling can be realized, and the efficiency is reduced.
Disclosure of Invention
The invention provides a method for recycling dust collection slag of a fused salt chlorination furnace, which aims to: through reasonable improvement of the prior art, the titanium-rich material in the titanium tetrachloride dust-collecting slag is effectively recovered, the treatment cost of the dust-collecting slag is reduced, valuable resources are recovered, and the process flow is shortened.
The technical scheme adopted by the invention is as follows:
a method for recycling dust collection slag of a molten salt chlorination furnace comprises the following steps:
step 1: dissolving titanium tetrachloride dust collection slag in a hydrochloric acid solution to obtain a slurry:
step 2: separating concentrate and first tailings from the slurry through flotation;
and step 3: reselecting the concentrate through a table concentrator to obtain titanium concentrate, second tailings and second filtrate, and performing filter pressing on the first tailings to obtain first filtrate and coke-containing filter residue;
and 4, step 4: and carrying out MVR treatment on the first filtrate and the second filtrate.
In a preferable technical scheme, in the step 1, when the pH value of the hydrochloric acid solution is less than 1, the pH value is adjusted to be within the range of 2-2.5 by filling new water.
In the preferable technical scheme, the second tailings are used for extracting rare and precious metals, valuable resources are recycled, and the process cost is reduced.
In the preferred technical scheme, the first filtrate and the second filtrate are subjected to MVR treatment for recovering NaCl, and the treated filtrate is returned to the chlorination furnace for secondary utilization.
In the preferable technical scheme, the concentration of the pulping material is between 20 and 25 percent, and the PH is less than 1.
In the preferred technical scheme, the ratio of the feeding speed of the pulping material to the feeding speed of the washing liquid of the shaking table in the gravity separation process of the shaking table is 3:1.
In the preferred technical scheme, the coke content of the coke-containing filter residue obtained by filter pressing the first tailings is more than 80%.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
different from the method directly used as slag treatment in the prior art, the method solves the technical problems that titanium coke is difficult to separate and rare and precious metals are difficult to recover in the prior art by means of table concentrator reselection, flotation, filter pressing and the like, in the technical scheme, the flotation is selected for first-step coke separation, a flotation agent and a catching agent with higher efficiency under an acidic condition are selected, and through experimental results, the coke content of the flotation tailings after coke filter pressing is more than 80 percent, so that the flotation tailings can be sold and economic benefits are generated; the flotation concentrate contains about 18 percent of titanium and the balance of aluminum, silicon and a small amount of vanadium, scandium and niobium; the grade of the obtained titanium concentrate reaches over 88 percent, the yield is 90 percent, the precious metals enriched in the obtained tailings reach the extraction recovery standard, and the wastewater finally enters MVR water for treatment and reaches the wastewater reuse standard; compared with the traditional recovery process, the invention shortens the process flow and improves the treatment efficiency.
Drawings
The invention will now be described, by way of example, with reference to the accompanying drawings, in which:
FIG. 1 is a process flow chart of the method for recovering the dust-collecting slag of the molten salt chlorination furnace
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all the embodiments. The components of embodiments of the present application, generally described and illustrated in the figures herein, may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present application, as presented in the figures, is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present application without making any creative effort, shall fall within the protection scope of the present application.
The present invention will be described in detail with reference to fig. 1.
Fig. 1 is a process flow diagram of a recovery method of dust-collecting slag of a molten salt chlorination furnace, which is used for realizing efficient energy-saving recovery of the dust-collecting slag of the molten salt chlorination furnace and reducing resource waste, and as shown in the figure, the recovery method of the dust-collecting slag of the molten salt chlorination furnace comprises the following steps:
step 1: dissolving titanium tetrachloride dust collection slag in a hydrochloric acid solution to obtain a slurry:
step 2: separating concentrate and first tailings from the slurry through flotation;
and step 3: reselecting the concentrate through a table concentrator to obtain titanium concentrate, second tailings and second filtrate, and performing filter pressing on the first tailings to obtain first filtrate and coke-containing filter residue with the coke content of more than 80%;
and 4, step 4: and carrying out MVR treatment on the first filtrate and the second filtrate.
In the step 1, when the acidity of the hydrochloric acid solution is too low (PH is less than 1), new water is required to be added for regulating the PH value to be within the range of 2-2.5 through material balance, and then a good pulping effect can be achieved.
In the step 2, the concentration of the pulping material is 20-25%, the pH is less than 1, the effect of the flotation agent added in the flotation process is better under the condition of strong acid, when the pH is more than 1.3, the flotation efficiency reaches 45%, and when the pH is less than or equal to 1, the flotation efficiency can reach 78% at most.
In the step 3, the second tailings are subjected to an extraction process to extract rare and precious metals such as vanadium, scandium and niobium, valuable resources are recycled, and the process cost is reduced.
Further, the ratio of the feeding speed of the pulping material in the table concentrator gravity separation process to the feeding speed of the table concentrator flushing liquid is 3:1, the ratio of the output and the feed rates of the pilot experiment is about 2.8, the experiment is widened to 3.
In the step 4, the first filtrate and the second filtrate are subjected to MVR treatment for recovering NaCl, and the treated filtrate is returned to the chlorination furnace for secondary utilization.
Wherein, the first filtrating behind the tailing filter pressing and partly second filtrating behind the gravity concentration of concentrate shaking table are used as the washing liquid circulation of shaking table and are used, can reduce the water consumption water economy resource and the cost of whole processing procedure.
The above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (7)

1. The method for recycling the dust collection slag of the molten salt chlorination furnace is characterized by comprising the following steps of:
step 1: dissolving titanium tetrachloride dust collection slag in a hydrochloric acid solution to obtain a slurry:
and 2, step: separating concentrate and first tailings from the slurry through flotation;
and step 3: reselecting the concentrate through a table concentrator to obtain titanium concentrate, second tailings and second filtrate, and performing filter pressing on the first tailings to obtain first filtrate and coke-containing filter residue;
and 4, step 4: and carrying out MVR treatment on the first filtrate and the second filtrate.
2. The method for recovering the dust collection slag of the molten salt chlorination furnace as claimed in claim 1, wherein in the step 1, when the pH of the hydrochloric acid solution is less than 1, the pH value is adjusted to be in the range of 2-2.5 by filling fresh water.
3. The method for recovering the dust collection slag of the molten salt chlorination furnace according to claim 1, wherein the second tailings are used for rare and precious metal extraction.
4. The method for recycling the dust collection slag of the molten salt chlorination furnace as claimed in claim 1, wherein the first filtrate and the second filtrate are subjected to MVR treatment for recycling NaCl, and the treated filtrate is returned to the chlorination furnace for secondary utilization.
5. The method for recycling the dust collection slag of the molten salt chlorination furnace according to claim 1, wherein the concentration of the pulping slurry is between 20% and 25%, and the pH value is less than 1.
6. The method for recycling the dust collection slag of the molten salt chlorination furnace as claimed in claim 1, wherein the ratio of the feeding rate of the pulping material to the feeding rate of the table washing liquid in the table reselection process is 3:1.
7. the method for recycling the dust collection slag of the molten salt chlorination furnace according to claim 1, wherein the coking rate of the coking-containing filter residue obtained by filter pressing of the first tailings is more than 80%.
CN202211182521.4A 2022-09-27 2022-09-27 Method for recycling dust collection slag of fused salt chlorination furnace Pending CN115475696A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202211182521.4A CN115475696A (en) 2022-09-27 2022-09-27 Method for recycling dust collection slag of fused salt chlorination furnace

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202211182521.4A CN115475696A (en) 2022-09-27 2022-09-27 Method for recycling dust collection slag of fused salt chlorination furnace

Publications (1)

Publication Number Publication Date
CN115475696A true CN115475696A (en) 2022-12-16

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