CN110616320B - Method for desiliconizing silicon-containing ore or slag - Google Patents

Method for desiliconizing silicon-containing ore or slag Download PDF

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CN110616320B
CN110616320B CN201910876750.8A CN201910876750A CN110616320B CN 110616320 B CN110616320 B CN 110616320B CN 201910876750 A CN201910876750 A CN 201910876750A CN 110616320 B CN110616320 B CN 110616320B
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silicon
solid
slag
leaching
nitric acid
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CN110616320A (en
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马保中
王成彦
曹志河
邢鹏
陈永强
张文娟
荆乾坤
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University of Science and Technology Beijing USTB
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/065Nitric acids or salts thereof
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/006Wet processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/006Wet processes
    • C22B7/007Wet processes by acid leaching
    • 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

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  • Environmental & Geological Engineering (AREA)
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  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Refinement Of Pig-Iron, Manufacture Of Cast Iron, And Steel Manufacture Other Than In Revolving Furnaces (AREA)

Abstract

The invention discloses a method for desiliconizing silicon-containing ores or slags, which belongs to the field of nonferrous metallurgy and comprises the steps of pressurizing by using nitric acid to activate silicon, controlling the concentration of the nitric acid to be 150-300 g/L and the leaching temperature to be 180-220 ℃, adding 85% phosphoric acid into activated slags according to the solid-to-liquid ratio of 1: 0.5-1: 2g/m L, fully stirring, placing the activated slags in a muffle furnace at 220-260 ℃ for pretreatment, and leaching pretreated materials with water to remove and separate silicon.

Description

Method for desiliconizing silicon-containing ore or slag
Technical Field
The invention belongs to the field of nonferrous metallurgy, and particularly relates to a method for desiliconizing silicon-containing ores or slags.
Background
At present, a plurality of metallurgical original ores and leaching slag contain a certain amount of silicon, wherein the silicon exists in the form of silicon dioxide and silicate, the quality of minerals is not high due to the existence of the silicon, the existence of the silicon must be considered in the mineral processing process, the technical difficulty and the processing cost of mineral utilization are further increased, and a general and efficient method for removing the silicon does not exist at present. Patent CN 105734265A proposes a method for removing silicon from molybdenum concentrate, in which sodium carbonate is mixed and ground with molybdenum concentrate. The method can well remove the silicon in the molybdenum concentrate, but has high energy consumption and low silicon removal rate. The patent CN 107857489A adopts an activating roasting reselection process for the magnesite to carry out desiliconization, and the process has a good removing effect on the silicon dioxide with larger granularity in the magnesite, but has a poor removing effect on the silicon dioxide with smaller granularity and other silicates, and has a long flow path and complex operation.
In conclusion, no generally applicable method for removing silicon from the original ore and the leached slag containing silicon is available at present, the efficient removal of silicon cannot be realized, and the defects of high energy consumption, long flow, complex operation and the like exist. The invention provides a method for removing silicon from silicon-containing ores or slags, which is characterized in that silicon is activated and transformed by utilizing the strong oxidizing property of nitric acid pressurization, and then the silicon in the silicon-containing ores or slags is effectively removed by utilizing phosphoric acid pretreatment and water immersion.
Disclosure of Invention
The invention provides a method for removing silicon from silicon-containing ores or slags, which comprises the steps of transforming silicon by utilizing the strong oxidizing property of nitric acid pressurization activation, then utilizing phosphoric acid for pretreatment, water leaching and drying to obtain the desilication slag.
The purpose of the invention is realized by the following technical scheme:
a method of desiliconizing a silicon-containing ore or slag comprising the steps of:
step one, nitric acid activation transformation: adding nitric acid with a certain concentration into the silicon-containing ore or slag, carrying out activation transformation, and carrying out liquid-solid separation on the transformed ore pulp to obtain leachate and activated slag;
step two, pretreatment of phosphoric acid: adding phosphoric acid into the activated slag obtained in the first step according to a certain solid-to-liquid ratio, fully stirring, and placing in a muffle furnace to complete pretreatment;
step three, water leaching and desiliconization: and (4) leaching the pretreated material in the step two by using hot water for desiliconization, and then carrying out solid-liquid separation to realize the removal of silicon in the silicon-containing ore or slag.
Further, during the activation transformation of nitric acid in the first step, the concentration of the nitric acid is 150-300 g/L, the solid-to-liquid ratio is 1: 2-1: 5g/m L, the leaching temperature is 180-220 ℃, the leaching time is 1-4 h, and the stirring speed is 350-600 rpm.
Further, in the step of phosphoric acid pretreatment, 85% phosphoric acid is mixed with the leaching residue according to the solid-to-liquid ratio of 2: 1-1: 2g/m L.
Further, the temperature is 220-260 ℃ and the time is 0.5-2 h during the phosphoric acid pretreatment in the step.
Further, when the water leaching desiliconization is carried out in the third step, the water leaching temperature is 60-90 ℃, the solid-to-liquid ratio is 1: 2-1: 5g/m L, the leaching time is 0.5-2 h, and the stirring speed is 250-500 rpm.
According to the technical scheme provided by the invention, the method for desiliconizing the silicon-containing ores or slag provided by the embodiment of the invention has the advantages of short flow, easiness in operation and capability of efficiently removing silicon.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
FIG. 1 is a flow diagram of the present invention for desilication from silicon-containing ores or slags.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without inventive step, are within the scope of the present invention.
The process of the present invention for desiliconizing siliceous ores or slags is described in detail below.
A process for the desilication of silicon-containing ores or slags, comprising the steps of:
step one, nitric acid activation transformation, namely adding nitric acid with initial acidity of 150-300 g/L into certain siliceous slag, wherein the solid-liquid ratio is 1: 2-1: 5g/m L, controlling the reaction conditions that the leaching temperature is 180-220 ℃, the leaching time is 1-4 h, and the stirring speed is 350-600 rpm, and completing the liquid-solid separation of activated ore pulp to obtain leachate and activated slag.
And step two, phosphoric acid pretreatment, namely adding 85% phosphoric acid into the leaching residue obtained in the step one according to a solid-to-liquid ratio of 2: 1-1: 2g/m L, fully stirring, and then placing in a muffle furnace at 220-260 ℃ for pretreatment for 0.5-2 h.
And step three, water leaching desiliconization, namely putting the material pretreated in the step two into hot water at the temperature of 60-90 ℃, wherein the solid-to-liquid ratio is 1: 2-1: 5g/m L, the leaching time is 0.5-2 h, the stirring speed is 250-500 rpm, carrying out solid-liquid separation, and drying to obtain desiliconized slag.
The technical scheme shows that: the invention provides a method for desiliconizing from silicon-containing ores or slag, which comprises the steps of pressurizing, activating and transforming by nitric acid, then converting insoluble silicon into soluble substances by utilizing phosphoric acid pretreatment, and finally removing silicon by water immersion.
The method for desiliconizing from the silicon-containing ore or slag provided by the invention has the following advantages:
(1) the method for desiliconizing from the silicon-containing ore or slag adopts nitric acid to perform pressure activation transformation, and has low cost and simple operation.
(2) The invention realizes the conversion of insoluble silicon into soluble substances by the pretreatment of phosphoric acid, and removes the silicon by simple water immersion.
(3) The invention fully utilizes the characteristics of silicon and efficiently removes the silicon from the silicon-containing ores or slag.
(4) The invention has the advantages of no alkali in the whole process, less reagent consumption, simple operation, short process and small pressure on the environment.
In order to more clearly show the technical scheme and the technical effects provided by the invention, the method for desiliconizing the silicon-containing ore or slag provided by the invention is described in detail by using specific examples.
Example 1
As shown in figure 1, a method for desiliconizing silicon-containing ores or slag comprises the steps of adding nitric acid with initial acidity of 150 g/L into certain silicon-containing ores, carrying out nitric acid pressurization activation under the conditions that the activation temperature is 180 ℃, the activation time is 1h, the liquid-solid ratio is 1:3g/m L and the stirring speed is 500rpm, drying activated slag after solid-liquid separation, mixing the dried activated slag with phosphoric acid with the concentration of 85% according to the solid-liquid ratio of 1:1g/m L, carrying out water immersion after the pretreatment is finished, carrying out water immersion under the conditions that the water temperature is 80 ℃, the solid-liquid ratio is 1:5g/m L and the stirring speed is 500rpm, carrying out solid-liquid separation and drying to obtain desiliconized slag.
Example 2
As shown in figure 1, a method for desiliconizing silicon-containing ores or slag comprises the steps of adding nitric acid with initial acidity of 200 g/L into certain silicon-containing slag, performing nitric acid pressure activation under the conditions that the activation temperature is 210 ℃, the activation time is 4 hours, the liquid-solid ratio is 1:2g/m L, the stirring speed is 600rpm, performing solid-liquid separation, drying the activated slag, mixing the dried activated slag with phosphoric acid with the concentration of 85% according to the solid-liquid ratio of 2:1g/m L, performing water immersion at the pretreatment temperature of 220 ℃ for 1 hour, performing solid-liquid separation after the pretreatment, and drying to obtain desiliconized slag, wherein the water temperature is 90 ℃, the solid-liquid ratio is 1:5g/m L, the time is 1 hour, and the stirring speed is 250 rpm.
Example 3
As shown in figure 1, a method for desiliconizing silicon-containing ores or slag comprises the steps of adding nitric acid with initial acidity of 250 g/L into certain silicon-containing ores, carrying out nitric acid pressure activation under the conditions that the activation temperature is 200 ℃, the activation time is 3 hours, the liquid-solid ratio is 1:5g/m L, the stirring speed is 400rpm, carrying out solid-liquid separation, drying activated slag, mixing the dried activated slag with phosphoric acid with the concentration of 85% according to the solid-liquid ratio of 3:2g/m L, carrying out pretreatment at the temperature of 250 ℃ for 0.5 hour, carrying out water immersion after the pretreatment, carrying out water temperature of 60 ℃, the solid-liquid ratio of 1:2g/m L, the time of 5 hours, and the stirring speed of 300rpm, carrying out solid-liquid separation, and drying to obtain desiliconized slag.
Example 4
As shown in figure 1, a method for desiliconizing silicon-containing ores or slags comprises the steps of adding nitric acid with initial acidity of 300 g/L into certain silicon-containing slags, carrying out nitric acid pressurization activation under the conditions that the activation temperature is 190 ℃, the activation time is 2 hours, the liquid-solid ratio is 1:2g/m L, the stirring speed is 350rpm, carrying out solid-liquid separation, drying the activated slags, mixing the dried activated slags with 85% phosphoric acid according to the solid-liquid ratio of 1:2g/m L, carrying out pretreatment at 230 ℃ for 1.5 hours, carrying out water immersion after the pretreatment is finished, carrying out water temperature of 60 ℃, the solid-liquid ratio of 1:3g/m L, the time is 1 hour, and the stirring speed is 450rpm, carrying out solid-liquid separation, and drying to obtain the desiliconized slags.
Example 5
As shown in figure 1, a method for desiliconizing silicon-containing ores or slag comprises the steps of adding nitric acid with initial acidity of 220 g/L into certain silicon-containing ores, carrying out nitric acid pressurization activation at an activation temperature of 220 ℃, an activation time of 2h, a liquid-solid ratio of 1:3g/m L and a stirring speed of 550rpm, drying activated slag after solid-liquid separation, mixing the dried activated slag with phosphoric acid with the concentration of 85% according to the solid-liquid ratio of 1:1g/m L, carrying out water immersion at a pretreatment temperature of 260 ℃ for 2h, carrying out water immersion at a water temperature of 70 ℃, a solid-liquid ratio of 1:4g/m L and a stirring speed of 0.5h after the pretreatment is finished, carrying out solid-liquid separation, and drying to obtain desiliconized slag.
In conclusion, the embodiment of the invention can successfully remove silicon in the silicon-containing ore or slag through phosphoric acid pretreatment and water leaching after nitric acid pressure activation transformation, thereby realizing effective impurity removal and separation.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (1)

1. A method of desiliconizing a silicon-containing ore or slag comprising the steps of:
step one, nitric acid activation transformation: adding nitric acid with a certain concentration into the silicon-containing ore or slag, carrying out activation transformation, and carrying out liquid-solid separation on the transformed ore pulp to obtain leachate and activated slag;
step two, pretreatment of phosphoric acid: adding phosphoric acid into the activated slag obtained in the first step according to a certain solid-to-liquid ratio, fully stirring, and placing in a muffle furnace to complete pretreatment;
step three, water leaching and desiliconization: leaching the pretreated material in the second step by using hot water for desiliconization, and then carrying out solid-liquid separation to realize the removal of silicon in the silicon-containing ore or slag;
when the nitric acid is activated and transformed in the first step, the concentration of the nitric acid is 150-300 g/L, the solid-to-liquid ratio is 1: 2-1: 5g/m L, the leaching temperature is 180-220 ℃, the leaching time is 1-4 h, and the stirring speed is 350-600 rpm;
wherein, when the second phosphoric acid is pretreated, 85 percent phosphoric acid is mixed with the leaching residue according to the solid-to-liquid ratio of 2: 1-1: 2g/m L;
wherein, the temperature is 220-260 ℃ and the time is 0.5-2 h when the phosphoric acid is pretreated in the second step;
and when the desiliconization is carried out by water leaching in the third step, the water leaching temperature is 60-90 ℃, the solid-to-liquid ratio is 1: 2-1: 5g/m L, the leaching time is 0.5-2 h, and the stirring speed is 250-500 rpm.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5587103A (en) * 1996-01-17 1996-12-24 Harris Corporation Composition, and method for using same, for etching metallic alloys from a substrate
CN102151614A (en) * 2010-12-15 2011-08-17 中国铝业股份有限公司 Method for dressing, desilicication and desulfuration of sulfur-containing bauxite
CN106904644A (en) * 2017-03-24 2017-06-30 大唐国际发电股份有限公司高铝煤炭资源开发利用研发中心 A kind of desiliconization flyash and its preparation method and application
CN108584971A (en) * 2018-05-04 2018-09-28 中国科学院过程工程研究所 A method of preparing high mode soluble silicate using gasification slag

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5587103A (en) * 1996-01-17 1996-12-24 Harris Corporation Composition, and method for using same, for etching metallic alloys from a substrate
CN102151614A (en) * 2010-12-15 2011-08-17 中国铝业股份有限公司 Method for dressing, desilicication and desulfuration of sulfur-containing bauxite
CN106904644A (en) * 2017-03-24 2017-06-30 大唐国际发电股份有限公司高铝煤炭资源开发利用研发中心 A kind of desiliconization flyash and its preparation method and application
CN108584971A (en) * 2018-05-04 2018-09-28 中国科学院过程工程研究所 A method of preparing high mode soluble silicate using gasification slag

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