WO2019148901A1 - Procédé de traitement de laitier de chrome par calcination par chloration en combinaison avec une minéralisation hydrothermale - Google Patents

Procédé de traitement de laitier de chrome par calcination par chloration en combinaison avec une minéralisation hydrothermale Download PDF

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Publication number
WO2019148901A1
WO2019148901A1 PCT/CN2018/111616 CN2018111616W WO2019148901A1 WO 2019148901 A1 WO2019148901 A1 WO 2019148901A1 CN 2018111616 W CN2018111616 W CN 2018111616W WO 2019148901 A1 WO2019148901 A1 WO 2019148901A1
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Prior art keywords
chromium
slag
hydrothermal
residue
solid
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Ceased
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PCT/CN2018/111616
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English (en)
Chinese (zh)
Inventor
林璋
刘学明
刘炜珍
邓洪
胡建宏
林佳玮
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South China University of Technology SCUT
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South China University of Technology SCUT
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • C22B1/08—Chloridising roasting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/30—Obtaining chromium, molybdenum or tungsten
    • C22B34/32—Obtaining chromium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C22B7/008—Wet processes by an alkaline or ammoniacal leaching
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/04—Working-up slag
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the invention belongs to the technical field of chromium slag treatment, and particularly relates to a method for treating chromium residue by chlorination roasting combined with hydrothermal mineralization.
  • the chromium pollution is mainly derived from the chromium salt production and use industry, and is mainly based on the pollution of chromium-containing waste residue.
  • Calcium roasting and calcium-free roasting processes used in the production of chromium salts produce chromium-containing waste residues. Among them, the calcium roasting process will produce 2-3 tons of chromium slag per ton of product produced. Although calcium-free roasting significantly reduces the chromium slag emissions and the hexavalent chromium content, the risk remains. In view of this, in order to get rid of the pollution caused by chromium slag, some developed countries continue to compress chromium salt production capacity and import chromium salt products from developing countries.
  • the harmlessness of chromium slag is mainly the in-situ reduction/fixation of chromium slag to reduce its toxicity, and chromium is still in the slag.
  • chromium is still in the slag.
  • the trivalent chromium in the chromium residue after detoxification may still be reoxidized to hexavalent chromium under the action of long-term oxidation conditions in the environment or by the action of manganese oxidizing bacteria, and has secondary toxicity.
  • chromium slag or industrial chrome-containing solid waste
  • chromium slag or industrial chrome-containing solid waste
  • the chlorination roasting method is mainly used in the metallurgical industry.
  • the chlorine element is chemically active and has a wide range of applications. Under certain conditions, it is easier to react with most metals or compounds such as metal oxides to form metal chlorides.
  • Other metal compounds such as oxides, sulfides, etc.
  • metal chlorides are easily soluble in water, ethanol and other solvents, relatively low melting point, easy to volatilize, etc., and for different metals, the degree of oxidation is different and There are significant differences in the physicochemical properties of the resulting metal-vaporized.
  • the chlorination roasting method is to convert the target metal component in the mineral raw material into a corresponding chloride by using a chlorinating agent such as chlorine gas, hydrogen chloride or solid chloride salt in the roasting process, and to achieve the target metal according to the characteristics of the above metal chloride
  • a chlorinating agent such as chlorine gas, hydrogen chloride or solid chloride salt in the roasting process
  • the high-temperature chlorination roasting method can be used to directly separate the metal from the gangue in the form of a gas phase or a molten phase, and the refining mineral raw material can be purified by other extraction methods such as infiltration.
  • the chlorination roasting method has lower operating temperature than other pyrometallurgical methods and saves energy; finally, the chlorination roasting method is beneficial to the comprehensive utilization of ore, and the metal separation efficiency is high; according to the difficulty of chlorination for different metals, The physicochemical properties of the produced metal chlorides are significantly different. Therefore, for the comprehensive utilization of low-grade components complex ore and waste tailings, the chlorination roasting method can be used to effectively separate the enriched metals, and the comprehensive utilization effect is obvious.
  • the current chlorination roasting method is mainly used for the separation and enrichment of metals in industrial metallurgical mineral raw materials. There has not been any report on the combined treatment of chlorination roasting with hydrothermal mineralization.
  • the Chinese patent "Recycling Process for Treatment of Chromium Slag and Wastewater” (CN102699006A) takes into account the recovery of chromium and the reuse of solid slag. Under normal temperature conditions, the chromium slag is almost completely dissolved with acid, and then different precipitants are added separately. The mixed ions in the solution are precipitated and separated, but this method requires a large amount of chemical reagents such as an acid and a precipitant, and the process is complicated and the treatment cost is high.
  • a method for treating chrome slag by chlorination roasting combined with hydrothermal mineralization comprises the following steps:
  • step (2) adding the fine powder after the step (1) is added to the hydrothermal reactor, adding a mineralizer aqueous solution, hydrothermal mineralization reaction at a temperature of 30 to 250 ° C for 2 to 24 hours;
  • step (3) The mixed liquid obtained in the step (2) is cooled and allowed to stand to obtain a chromium-containing supernatant liquid and solid residue, and the solid residue is washed with water and dried to obtain detoxified chromium residue, and the chromium-containing supernatant is used for production. Or recycle chrome.
  • the chloride salt in step (1) is sodium chloride or calcium chloride.
  • the mass ratio of the chromium slag to the chloride salt is 1: (0.5 to 1.5).
  • the mineralizer described in the step (2) is at least one of sodium carbonate and sodium hydrogencarbonate; and the concentration of the mineralizer aqueous solution is 0.5 to 1.5 mol/L.
  • the solid-liquid ratio of the sieved fine powder and the mineralizer aqueous solution in the step (2) is 1: (0.5 to 10) (w/w).
  • the step of recovering the chromium treatment in the step (3) is: adding a reducing agent to reduce the hexavalent chromium of the solution to trivalent chromium, and then adding a precipitating agent NaOH to produce a Cr(OH) 3 precipitate for recovery.
  • the reducing agent includes sodium sulfide, sodium hydrogen sulfite, and the like.
  • the leaching of hexavalent chromium includes not only the surface free state and the leaching of the adsorbed hexavalent chromium, but also the slow diffusion and dissolution of the soluble hexavalent chromium trapped inside the solid particles.
  • the package leads to a large mass transfer resistance, and the hexavalent chromium in the sandwich state is difficult to leaching in a short time.
  • the chlorination roasting method can be selected to react with most metals or metal compounds including chromium at high temperature to form corresponding chlorides, which have the characteristics of lower melting point and can be released inside the microscopic solid particles to reach the metal materials including chromium and
  • the purpose of separation of other solid phase impurities is to improve chromium separation and refining efficiency, and ultimately increase the recovery rate of chromium.
  • the subsequent mineralizer hydrothermal treatment causes a small amount of trivalent chromium in the chromium slag to be oxidized to hexavalent chromium, and it is easier to enter the solution with the presence of dichromate.
  • the invention combines the chlorination roasting technology in industrial metallurgy to treat the chromium slag, solves the problem that the hexavalent chromium in the chromium slag is difficult to separate from the internal solid particles (including aluminosilicate, iron oxide, etc.), and improves the separation of chromium. Efficiency and recycling efficiency.
  • the treated slag leaching hexavalent chromium content is lower than the national standard (HJ/T301-2007) general industrial solid waste residue, and the process is simple, suitable for large-scale industrial production processes, large processing capacity, high recovery rate, detoxification The effect is good, with high social and economic benefits.
  • FIG. 1 is a schematic flow chart of a chlorination roasting combined with hydrothermal mineralization treatment of chromium slag according to an embodiment of the present invention.
  • FIG. 1 A method for chlorination roasting combined with hydrothermal mineralization to treat chromium slag according to the embodiment is shown in FIG. 1 . Specific steps are as follows:
  • the mixture obtained in the step (2) is naturally cooled to room temperature and allowed to stand for 12 hours to obtain a chromium-containing supernatant liquid and solid residue, and the solid residue is separated from the chromium-containing supernatant by filtration, and the solid residue is washed with water, dried and dried.
  • the chromium-containing supernatant is reused in the production, or collected in a wastewater treatment station for reduction, recovery, purification treatment (adding a reducing agent (such as sodium sulfide, sodium hydrogen sulfite), the solution
  • the hexavalent chromium is reduced to trivalent chromium, and the precipitated NaOH is added to produce Cr(OH) 3 precipitate for recovery.
  • the water can reach the national drainage standard). Water can be recycled in the system throughout the process.
  • the original chromium residue of the present embodiment has a hexavalent chromium concentration of 740 mg/L, and the treated residue has a hexavalent chromium concentration of 0.975 mg/L.
  • FIG. 1 A method for chlorination roasting combined with hydrothermal mineralization to treat chromium slag according to the embodiment is shown in FIG. 1 . Specific steps are as follows:
  • the mixture obtained in the step (2) is naturally cooled to room temperature and allowed to stand for 0.5 h to obtain a chromium-containing supernatant liquid and solid residue, and the solid residue is separated from the chromium-containing supernatant by filtration, and the solid residue is washed with water and dried.
  • the chromium-containing supernatant is reused in production, or collected in a wastewater treatment station for reduction, recovery, and purification treatment (adding a reducing agent (such as sodium sulfide, sodium hydrogen sulfite),
  • the solution of hexavalent chromium is reduced to trivalent chromium, and the precipitated NaOH is added to produce Cr(OH) 3 precipitate for recovery.
  • the water can reach the national drainage standard). Water can be recycled in the system throughout the process.
  • the original chromium residue of the present embodiment has a hexavalent chromium concentration of 763 mg/L, and the treated residue has a hexavalent chromium concentration of 1.025 mg/L.
  • FIG. 1 A method for chlorination roasting combined with hydrothermal mineralization to treat chromium slag according to the embodiment is shown in FIG. 1 . Specific steps are as follows:
  • the mixture obtained in the step (2) is naturally cooled to room temperature and allowed to stand for 0.5 h to obtain a chromium-containing supernatant liquid and solid residue, and the solid residue is separated from the chromium-containing supernatant by filtration, and the solid residue is washed with water and dried.
  • the chromium-containing supernatant is reused in production, or collected in a wastewater treatment station for reduction, recovery, and purification treatment (adding a reducing agent (such as sodium sulfide, sodium hydrogen sulfite),
  • the solution of hexavalent chromium is reduced to trivalent chromium, and the precipitated NaOH is added to produce Cr(OH) 3 precipitate for recovery.
  • the water can reach the national drainage standard). Water can be recycled in the system throughout the process.
  • the original chromium residue of the present embodiment has a hexavalent chromium concentration of 752 mg/L, and the treated residue has a hexavalent chromium concentration of 0.850 mg/L.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Metallurgy (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Processing Of Solid Wastes (AREA)
  • Treatment Of Water By Oxidation Or Reduction (AREA)

Abstract

L'invention concerne un procédé de traitement de laitier de chrome par calcination par chloration en combinaison avec une minéralisation hydrothermale, comprenant les étapes consistant à : ajouter sel de chlorure dans du laitier de chrome et mélanger le sel de chlorure et le laitier de chrome à uniformiser, élever la température à 400 à 1000 °C pour effectuer un traitement de calcination à haute température pendant 0,5 à 12 h, et broyer et tamiser après refroidissement ; ajouter la poudre fine obtenue à un réacteur hydrothermique, ajouter une solution aqueuse de minéralisation, et effectuer une réaction de minéralisation hydrothermique à une température de 30 à 250 °C pendant 2 à 24 h ; et refroidir le mélange et le laisser reposer pour obtenir un surnageant contenant du chrome et du laitier solide, laver le laitier solide avec de l'eau et sécher le laitier solide pour obtenir du laitier de chrome détoxifié, et réutiliser le surnageant contenant du chrome pour produire ou réaliser un traitement de récupération de chrome. Le laitier de chrome est traité par technologie de calcination de chloration en métallurgie industrielle en combinaison avec une minéralisation hydrothermale, résolvant le problème de séparation du chrome hexavalent des particules solides internes dans le laitier de chrome, améliorant l'efficacité de séparation et l'efficacité de récupération du chrome, ce qui procure des avantages sociaux et économiques élevés.
PCT/CN2018/111616 2018-01-30 2018-10-24 Procédé de traitement de laitier de chrome par calcination par chloration en combinaison avec une minéralisation hydrothermale Ceased WO2019148901A1 (fr)

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CN201810087145.8A CN108330274B (zh) 2018-01-30 2018-01-30 一种氯化焙烧联合水热矿化处理铬渣的方法

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CN108330274B (zh) * 2018-01-30 2019-11-15 华南理工大学 一种氯化焙烧联合水热矿化处理铬渣的方法
CN109554536A (zh) * 2018-11-23 2019-04-02 华南理工大学 一种真空氯化焙烧处理重金属危废的装置及方法
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CN109280777A (zh) * 2018-11-29 2019-01-29 华南理工大学 一种氯化焙烧法选择性回收电镀污泥中重金属的方法
CN109762991B (zh) * 2019-01-22 2019-11-29 福州大学 一种含铬电镀污泥中重金属选择性分离回收工艺
CN112853112A (zh) * 2021-01-09 2021-05-28 中新国际联合研究院 一种实现全回收铬渣中铬的方法
CN113620318B (zh) * 2021-07-31 2022-10-25 华南理工大学 一种氯化法处理含铬芒硝废盐的方法
CN117660750B (zh) * 2023-11-25 2026-05-05 重庆理工大学 一种通过还原碱焙烧强化无钙焙烧铬渣梯级分离及资源化利用的方法
CN118122758A (zh) * 2024-04-22 2024-06-04 西安建筑科技大学 一种强化铬渣在光照环境下稳定性的方法

Citations (6)

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GB509368A (en) * 1937-06-15 1939-07-14 Great Western Electro Chemical Co Method of chlorinating finely divided chromite
CN101209873A (zh) * 2006-12-27 2008-07-02 中国科学院福建物质结构研究所 含六价铬废渣的铬分离回收法
CN101746828A (zh) * 2008-12-09 2010-06-23 西南科技大学 氯化离析法回收铬渣中铬的方法与工艺
CN102191374A (zh) * 2010-03-10 2011-09-21 中国科学院过程工程研究所 传统铬渣资源化的方法
CN106011482A (zh) * 2016-06-30 2016-10-12 华南理工大学 一种铬渣的铬资源回收和脱毒处理方法
CN108330274A (zh) * 2018-01-30 2018-07-27 华南理工大学 一种氯化焙烧联合水热矿化处理铬渣的方法

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CN106048239B (zh) * 2016-06-30 2018-07-20 华南理工大学 一种含六价铬废渣的资源循环再利用的处理方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB509368A (en) * 1937-06-15 1939-07-14 Great Western Electro Chemical Co Method of chlorinating finely divided chromite
CN101209873A (zh) * 2006-12-27 2008-07-02 中国科学院福建物质结构研究所 含六价铬废渣的铬分离回收法
CN101746828A (zh) * 2008-12-09 2010-06-23 西南科技大学 氯化离析法回收铬渣中铬的方法与工艺
CN102191374A (zh) * 2010-03-10 2011-09-21 中国科学院过程工程研究所 传统铬渣资源化的方法
CN106011482A (zh) * 2016-06-30 2016-10-12 华南理工大学 一种铬渣的铬资源回收和脱毒处理方法
CN108330274A (zh) * 2018-01-30 2018-07-27 华南理工大学 一种氯化焙烧联合水热矿化处理铬渣的方法

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