CN113120911B - Method for ultrasonically reinforcing and separating silicon and iron in copper smelting slag and preparing white carbon black by utilizing silicon - Google Patents
Method for ultrasonically reinforcing and separating silicon and iron in copper smelting slag and preparing white carbon black by utilizing silicon Download PDFInfo
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- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/126—Preparation of silica of undetermined type
- C01B33/128—Preparation of silica of undetermined type by acidic treatment of aqueous silicate solutions
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Abstract
The application relates to a method for separating silicon and iron in copper smelting slag by ultrasonic reinforcement and preparing white carbon black by utilizing silicon, belonging to the field of comprehensive utilization of industrial solid wastes. Firstly, crushing copper smelting slag to more than 90% and the granularity is smaller than 0.075mm, then realizing mineral phase conversion and separation in sodium hydroxide solution under the synergistic catalysis of sodium nitrate and ultrasonic waves, and carrying out solid-liquid separation and washing on a reaction product to obtain a filtering liquid and filter residues, wherein the filtering liquid is used for preparing white carbon black, and the main component of the filter residues is hematite and can be used for ironmaking operation. According to the application, sodium hydroxide and sodium nitrate are added into copper smelting slag, silicon in the slag is converted into sodium silicate under the condition of ultrasonic reinforcement, so that silicon in the copper smelting slag with complex structure and composition is separated from impurity elements such as iron, calcium, copper and the like in the slag, a white carbon black product with high added value is prepared, and after the white carbon black product is prepared, byproduct filter residues are directly used as high-quality iron-making raw materials for iron-making operation, thereby realizing the purpose of efficiently utilizing silicon and iron in the copper smelting slag.
Description
Technical Field
The application relates to the field of comprehensive utilization of industrial solid wastes, in particular to a method for separating silicon and iron in copper smelting slag by ultrasonic reinforcement and preparing white carbon black by utilizing silicon.
Background
Copper smelting slag is a main bulk solid waste in the copper metallurgy industry, and has a complex composition structure and extremely low comprehensive utilization rate. For many years, metallurgical enterprises always discard copper smelting slag in an open air environment, so that a large amount of land resources are occupied, toxic and harmful elements such as arsenic and lead in the slag and heavy metals such as nickel and cobalt in the slag can enter surface water systems and soil along with erosion of rainwater and surface runoff, and pollution is caused to water bodies, soil and crops. Since 1996, china has been the largest nonferrous metal producer worldwide, but the metal content in metallurgical raw materials is often not high, and is often accompanied or symbiotic with toxic elements such as lead, arsenic and the like, and a large amount of flux such as calcium oxide, silicon dioxide and the like is also needed to be matched in the smelting process, so that the yield of metallurgical slag is huge. In 2020, the production amount of refined copper reaches 1003 ten thousand tons, more than 2.5 tons of copper smelting slag is produced per ton of refined copper produced, one spot is visible in the quantity of copper metallurgical slag which is newly produced and accumulated in natural environment, and reports of heavy metal pollution of land, river and grain crops in southwest and south provinces are generated, so that solid waste produced in mining industry poses a great threat to the living environment of human beings.
The copper smelting slag contains mineral phase components such as magnetite, vitreous phase and iron olivine, wherein the amorphous vitreous phase and the iron olivine phase are main constituent phases, the proportion of the amorphous vitreous phase and the iron olivine phase is 45% +/-40% +/-and the proportion of iron in the vitreous phase, the iron olivine phase and the magnetite phase is 44.94%, 44.30% and 10.34% of the total iron in the slag respectively. FeO and SiO in copper smelting slag 2 The content of CaO is close to 80%, but the content of CaO is lower, and the composition difference of CaO and silicate cement building materials is larger, so that the cement cannot be directly used in a large amount in the building material industry, and can only be used as an auxiliary material in the building industry. Although recent studies report that the copper slag and other materials are matched to obtain excellent properties of the fired cement clinker (Qin Shouwan, shen Jianjun, wu Chunli. Application of slag, copper slag in cement production [ J)]Silicate notification, 2013,32 (4): 572-576,582.). However, alkaline substances such as ferric oxide in the copper slag and the like are combined with moisture and CO in the atmosphere 2 The chemical reaction is carried out to cause weathering and dissolution, and expansion is caused under alkaline environment, thus causing damage to buildings, and restricting the application of the chemical reaction in building materials (Hu Chunqing, heng Xiaozhi, national security. Investigation and research on the damage to buildings caused by alkaline expansion of steel copper slag [ J)]Geotechnical foundation 2000,14 (1): 35-38; wang Feng analysis of concrete pop accident cause of certain school [ J ]]Concrete and cement products, 2011 (12): 53-55.).
The utilization method of iron in copper smelting slag mainly comprises the methods of high-temperature oxidation, magnetic separation to obtain iron concentrate, high-temperature melting reduction, enrichment and iron extraction, high Wen Meiji direct reduction and the like. The main process of the high-temperature oxidation and magnetic separation method is as follows: blowing oxygen-enriched air or oxygen into high-temperature molten copper smelting slag to carry out modification treatment, promoting iron oxide phase transfer, migration, enrichment and crystallization in slag, and realizing coarsening of Fe 3 O 4 The grain size of the phase is favorable for magnetic separation and iron recovery. The iron concentrate containing 54 percent of iron can be obtained through high-temperature oxidation and magnetic separation, and the recovery rate of iron is about 90 percent.
The process for high-temperature melting copper oxide slag and enriching and extracting iron mainly comprises the following steps: adding calcium oxide into a copper smelting melt at 1350 ℃ and introducing oxygen to oxidize copper slag, firstly, adding the calcium oxide into the copper smelting meltConversion of iron component in fayalite to Fe 3 O 4 Then the iron concentrate is obtained through magnetic separation, the grade of the iron concentrate is above 61 percent, but the recovery rate of iron is about 70 percent (Liu Gang, zhu Rong, wang Changan, etc.. Test research of copper slag melting oxidation iron extraction [ J)]Chinese nonferrous metallurgy 2009, (1) 71-74; huang Zili, luo Fan, li Mi, et al, experimental investigation of recovery of iron from copper-smelting water quench slag [ J]Mineral protection and utilization 2009, (3) 51-54.). Adding certain slag former CaO into copper slag, reducing and smelting iron in the copper slag in a high-temperature molten state, clarifying slag phase and metal phase obtained by reduction, separating to obtain metal iron, wherein copper enters molten iron phase in the smelting reduction process, so that the copper content in molten iron is high, and the problem that copper is still effectively separated and removed in the molten iron worldwide is still solved, which is the disadvantage of the scheme (Li Lei, hu Jianhang, wang Hua. Thermodynamic analysis of reaction in the smelting reduction iron-making process of copper slag [ J ]]Material guide B,2011,25 (7): 114-117; hu Jianhang, wang Hua, liu Huili, etc. the crystal phase structure of copper slag at different calcining temperatures [ J]Instructions on Hunan university of science and technology (Nature science edition), 2011,26 (2): 97-100.).
Research on direct reduction of iron in copper slag at high temperature (1250 ℃) by using brown coal as reducing agent shows that Fe in slag 3 O 4 、2FeO·SiO 2 Can be directly reduced into iron, and the addition of 10% of calcium oxide by weight of copper slag can raise the reduction efficiency of iron in slag, and by controlling reduction temperature, reduction time and granularity of material, the goal of directional control of metal iron grain size and interface characteristic of metal iron in the reduced product can be reached, and the metal iron can be easily dissociated and separated by magnetic separation so as to obtain iron powder whose iron weight fraction is 92.05% (Yang Huifen, jing Lili, dangchun pavilion and direct reduction and magnetic separation recovery of iron component in copper slag [ J)]Chinese nonferrous metals journal 2011,21 (5): 1165-1170.).
The high temperature oxidation scheme converts iron compounds in the slag to Fe at temperatures up to 1350 DEG C 3 O 4 And then recovering iron resources in the slag through magnetic separation. The medium-low temperature oxidation process only relates to the oxidation of iron in fayalite phase in copper slag into magnetic iron oxide, and then magnetic separation into iron concentrate products. However, whether it is a high temperature oxidation or a medium and low temperature oxidation process, when the iron reaches the grade of acceptable iron concentrateThe recovery rate is not high, the iron in the copper slag is recovered in the form of magnetic ferric oxide, the amount of reducing agent consumed when entering a blast furnace for iron making operation is increased, and the energy consumption of the subsequent process is high. The high-temperature melting reduction requires a temperature above 1380 ℃, the direct reduction of coal base is up to 1250 ℃, and the high energy consumption is fatal hard injury. In addition, the reduction process consumes a great deal of carbon and also generates a great deal of greenhouse gas CO 2 。
In summary, the silicon in the copper smelting slag cannot be effectively utilized at present, and the utilization technology of iron in the slag has the defects of low recovery rate, high energy consumption and environmental pollution, and is not applied to industrial practice.
Disclosure of Invention
Aiming at the problems and the defects existing in the prior art, the application provides a method for ultrasonically reinforcing and separating silicon and iron in copper smelting slag and preparing white carbon black by utilizing silicon. By adding sodium hydroxide and sodium nitrate into copper smelting slag, silicon in the slag is converted into sodium silicate under the condition of ultrasonic reinforcement, so that silicon in the copper smelting slag with complex structure and composition is separated from impurity elements such as iron, calcium, copper and the like in the slag, and after a white carbon black product is prepared, byproduct filter residues are directly used as high-quality iron-making raw materials for iron-making operation, thereby realizing the purpose of efficiently utilizing the silicon and the iron in the copper smelting slag. The application is realized by the following technical scheme.
A method for separating silicon and iron in copper smelting slag by ultrasonic reinforcement and preparing white carbon black by utilizing silicon is characterized by comprising the following steps:
step 1, crushing: crushing copper smelting slag to obtain powdery copper smelting slag;
step 2, ultrasonic intensified leaching: weighing 100g of the powdery copper smelting slag obtained in the step 1, adding 400-800 mL of sodium hydroxide solution with the mass concentration of 20-60% into an ultrasonic pressurizing reaction kettle, adding sodium nitrate with the addition amount of 5-20% of the mass of the powdery copper smelting slag, stirring and reacting for 1.0-3.0 h at 120-200 ℃ under ultrasonic irradiation, and cooling the reactant to the temperature lower than 80 ℃ after the reaction is finished;
step 3, solid-liquid separation: carrying out solid-liquid separation and washing on the reaction product cooled in the step 2 to obtain a filtering liquid and filter residues;
step 4, aging: heating the filtering and washing liquid obtained in the step 3 to 80-90 ℃, adding 10-30% of dilute sulfuric acid solution under stirring to adjust the pH of the filtering and washing liquid to 2.5-3.5, continuously stirring and reacting for 1.0-2.0 h, and standing and ageing for 1.5-2.5 h after the reaction is finished to obtain an aged precipitate;
step 5, filtering: filtering and washing the precipitate obtained in the step 4 to obtain a filter cake;
step 6, drying: and (3) drying the filter cake obtained in the step (5) at 105-110 ℃ for 1-2 h to obtain the white carbon black.
By the method, sodium hydroxide and sodium nitrate are added into copper smelting slag, silicon in the slag is converted into sodium silicate under the condition of ultrasonic reinforcement, silicon in the copper smelting slag with complex structure and composition is separated from impurity elements such as iron, calcium, copper and the like in the slag, a white carbon black product is prepared, and a byproduct, namely high-quality raw material hematite, can be used for iron-making operation. The powder copper smelting slag is subjected to sodium nitrate and ultrasonic wave synergistic catalysis to realize mineral phase conversion and separation in sodium hydroxide solution, so that more than 98.0% of silicon dioxide in the copper smelting slag can be converted, enter a liquid phase, and carry out solid-liquid separation and washing on a reaction product, so that a white carbon black product with high added value is prepared, and the quality of the prepared white carbon black product meets the national grade A standard of white carbon black; the filter residue (by-product) obtained after separating silicon is a high-quality raw material which can be used for ironmaking operation, namely hematite.
The copper smelting slag comprises the following components in percentage by mass: fe 30-50% and SiO 2 25％～35％、CaO 1.0％～10.0％、MgO 1.0％～5.0％、Al 2 O 3 0.5％～5.0％、Cu 0.1％～1.0％、S 0.05％～1.0％。
The granularity of the crushed copper smelting slag in the step 1 is smaller than 0.075mm.
The main component of the filter residue in the step 3 is hematite, which is a high-quality iron-making raw material capable of being used for iron-making operation.
The method of the application realizes the purpose of efficiently utilizing silicon and iron in the copper smelting slag because the byproduct (the filter residue with hematite as the main component) can be directly used as a high-quality iron-making raw material for iron-making operation while silicon is separated from the copper smelting slag and the white carbon black product is prepared.
And (3) filtering in the step (5), namely filtering the aged precipitate, washing with 50mL of deionized water for three times, and washing with 50mL of absolute ethyl alcohol for three times to obtain the filter cake.
The beneficial effects of the application are as follows:
1. according to the application, silicon in slag is converted into sodium silicate under the condition of ultrasonic reinforcement, so that silicon in copper smelting slag with complex structure and composition is separated from impurity elements such as iron, calcium, copper and the like in slag, and the separated silicon is utilized to prepare a white carbon black product with high added value; after separating silicon from copper smelting slag, filtering residues are Fe 2 O 3 The content of Cu and S in the filter residue is lower than 0.5 percent as the main component, and the filter residue is a high-quality raw material which can be directly used for ironmaking operation, thereby realizing the technical effect of efficiently utilizing silicon and iron in the copper smelting slag.
2. The application can convert more than 99.0% of iron in the copper smelting slag into hematite phase, has high iron recovery rate, does not generate sulfur dioxide and greenhouse gases, and has environment-friendly process and low energy consumption.
3. According to the application, the silicon in the solid waste is utilized at a high value, the silicon utilization rate is more than 95.0%, and the quality of the prepared white carbon black product reaches the national standard.
4. The leaching rate of the silicon dioxide can be improved by more than 10% by the synergistic catalysis strengthening of sodium nitrate and ultrasound.
Drawings
FIG. 1 is a process flow diagram of the present application.
Fig. 2 is a mass percentage composition diagram of elements in the copper smelting slag of the present application.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the application. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present application. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
The application will be further described with reference to the following specific embodiments.
Example 1
As shown in fig. 1, the method for preparing white carbon black by utilizing silicon and iron in copper smelting slag through ultrasonic reinforcement separation comprises the following steps:
(1) Crushing copper smelting slag to more than 90% and with granularity smaller than 0.075mm, wherein the copper smelting slag comprises the following components in percentage by mass 2 32.5％、CaO 3.2％、MgO 1.5％、Al 2 O 3 0.5％、Cu 0.3％、S 0.4％。
(2) 100g of copper smelting slag with granularity smaller than 0.075mm, which is crushed to be more than 90%, is added into an ultrasonic pressurizing reaction kettle, 400mL of NaOH solution with mass concentration of 60% is added, 20g of industrial sodium nitrate is added, and the mixture is reacted for 2.0h under mechanical stirring and ultrasonic irradiation at the temperature of 180 ℃; after leaching, stopping heating, introducing cooling water to cool the solution to a temperature lower than 60 ℃, taking out ore pulp for solid-liquid separation, simultaneously washing filter residues with 50mL of hot water at 85 ℃ for three times to obtain 435mL of filter liquor, drying the filter residues in an oven at 120 ℃ for 2h, weighing to 65.2g, and adding Fe in the filter residues 2 O 3 The mass contents of Cu and S are 86.7%,0.45% and 0.31%, respectively, and can be directly used for ironmaking operation.
(3) Heating 435mL of the obtained filtrate and washing liquid to 80 ℃, adding 30% dilute sulfuric acid solution under stirring, adjusting the pH of the solution to 2.5, continuing to react for 1.0h under stirring, stopping stirring and aging for 2.5h, filtering, washing with 50mL of deionized water for three times, and washing with 50mL of absolute ethyl alcohol for three times to obtain the productThe filter cake is dried in a drying oven at 110 ℃ for 1.5h to obtain 31.1g of white carbon black product. The oil absorption value of the prepared white carbon black product is 2.2mL/g, and the specific surface area reaches 295.60m 2 And/g, meets the national A-grade standard of white carbon black.
Example 2
As shown in fig. 1, the method for preparing white carbon black by utilizing silicon and iron in copper smelting slag through ultrasonic reinforcement separation comprises the following steps:
(1) Crushing copper smelting slag to more than 90% and with granularity smaller than 0.075mm, wherein the copper smelting slag comprises the following components in percentage by mass 2 25％、CaO 1.0％、MgO 1.0％、Al 2 O 3 0.9％、Cu 0.4％、S 1.0％。
(2) 100g of copper smelting slag with granularity smaller than 0.075mm, which is crushed to be more than 90%, is added into an ultrasonic pressurizing reaction kettle, 700mL of NaOH solution with mass concentration of 20% is added, 15g of industrial sodium nitrate is added, and the mixture is reacted for 3.0h under mechanical stirring and ultrasonic irradiation at the temperature of 200 ℃; after leaching, stopping heating, introducing cooling water to cool the solution to a temperature lower than 80 ℃, taking out ore pulp for solid-liquid separation, simultaneously washing the filter cake with 50mL of 80 ℃ hot water for three times to obtain 730mL of filter liquor, drying the filter cake in an oven at 120 ℃ for 2h, weighing 73.5g, and adding Fe in the filter cake 2 O 3 The mass contents of Cu and S are 95.6%,0.48% and 0.48%, respectively, and can be directly used for ironmaking operation.
(3) And (3) heating 730mL of the obtained filtered and washed solution to 90 ℃, adding 10% of dilute sulfuric acid solution in an agitating state, wherein the adding amount is used for adjusting the pH of the solution to 3.5 as an end point, continuously agitating again to react for 2.0h, stopping agitating and aging for 1.5h, filtering, washing with 50mL of deionized water for three times, washing with 50mL of absolute ethyl alcohol for three times to obtain a filter cake, and drying the filter cake in a drying oven at 105 ℃ for 2.0h to obtain 24.25g of white carbon black product. The oil absorption value of the prepared white carbon black product is 2.5mL/g, and the specific surface area reaches 298.50m 2 And/g, meets the national A-grade standard of white carbon black.
Example 3
As shown in fig. 1, the method for preparing white carbon black by utilizing silicon and iron in copper smelting slag through ultrasonic reinforcement separation comprises the following steps:
(1) Crushing copper smelting slag to more than 90% and with granularity smaller than 0.075mm, wherein the copper smelting slag comprises the following components in percentage by mass 2 35％、CaO 10.0％、MgO 5.0％、Al 2 O 3 5.0％、Cu 0.2％、S 0.7％。
(2) 100g of copper smelting slag with granularity smaller than 0.075mm, which is crushed to be more than 90%, is added into an ultrasonic pressurizing reaction kettle, 800mL of NaOH solution with mass concentration of 30% is added, 10g of industrial sodium nitrate is added, and the mixture is reacted for 1.0h under the conditions of mechanical stirring and ultrasonic irradiation at 120 ℃; after leaching, stopping heating, introducing cooling water to cool the solution to a temperature lower than 60 ℃, taking out ore pulp for solid-liquid separation, simultaneously washing filter residues with 50mL of hot water at 85 ℃ for three times to obtain 836mL of filter liquor, drying the filter residues in an oven at 120 ℃ for 2h, weighing to 65.2g, and adding Fe in the filter residues 2 O 3 The mass contents of Cu and S are 65.0%,0.28% and 0.46%, respectively, and can be directly used for ironmaking operation.
(3) 836mL of the obtained filtrate and washing liquid is heated to 85 ℃, 20% dilute sulfuric acid solution is added under stirring, the addition is carried out to adjust the pH of the solution to 3.0 as an end point, stirring is continued to react for 1.5 hours, stirring and aging are stopped for 2.0 hours, filtration is carried out, 50mL of deionized water is used for three times of washing, 50mL of absolute ethyl alcohol is used for three times of washing to obtain a filter cake, and the filter cake is dried in a drying oven at 110 ℃ for 1.0 hour to obtain 33.6g of white carbon black product. The oil absorption value of the prepared white carbon black product is 2.8mL/g, and the specific surface area reaches 290.60m 2 And/g, meets the national A-grade standard of white carbon black.
Example 4
As shown in fig. 1, the method for preparing white carbon black by utilizing silicon and iron in copper smelting slag through ultrasonic reinforcement separation comprises the following steps:
(1) Crushing copper smelting slag to more than 90% and with granularity smaller than 0.075mm, wherein the copper smelting slag comprises the following components in percentage by mass 2 33.5％、CaO 6.0％、MgO 2.5％、Al 2 O 3 3.5％、Cu 0.1％、S 0.05％。
(2) Smelting copper with granularity smaller than 0.075mm and crushed to more than 90%100g of slag is added into an ultrasonic pressurizing reaction kettle, 500mL of NaOH solution with the mass concentration of 40% is added, 5g of industrial sodium nitrate is added, and the reaction is carried out for 1.5h under the conditions of mechanical stirring and ultrasonic irradiation at the temperature of 150 ℃; after leaching, stopping heating, introducing cooling water to cool the solution to a temperature lower than 60 ℃, taking out ore pulp for solid-liquid separation, simultaneously washing filter residues with 50mL of hot water at 85 ℃ for three times to obtain 532mL of filter liquor, drying the filter residues in an oven at 120 ℃ for 2h, weighing to 66.0g, and adding Fe in the filter residues 2 O 3 The mass contents of Cu and S are 86.1%,0.15% and 0.03%, respectively, and can be directly used for ironmaking operation.
(3) 532mL of the obtained filtrate and washing liquid is heated to 80 ℃, 15% dilute sulfuric acid solution is added under stirring, the addition is carried out to adjust the pH of the solution to 2.5 as an end point, stirring is continued to react for 2.0h, stirring and aging are stopped for 2.0h, filtration is carried out, 50mL of deionized water is used for three times of washing, 50mL of absolute ethyl alcohol is used for three times of washing to obtain a filter cake, and the filter cake is dried in a drying box at 110 ℃ for 1.5h to obtain 32.1g of white carbon black product. The oil absorption value of the prepared white carbon black product is 2.5mL/g, and the specific surface area reaches 290.80m 2 And/g, meets the national A-grade standard of white carbon black.
Example 5
As shown in fig. 1, the method for preparing white carbon black by utilizing silicon and iron in copper smelting slag through ultrasonic reinforcement separation comprises the following steps:
(1) Crushing copper smelting slag to more than 90% and with granularity smaller than 0.075mm, wherein the copper smelting slag comprises the following components in percentage by mass 2 33.5％、CaO 2.2％、MgO 1.5％、Al 2 O 3 2.8％、Cu 0.2％、S 0.3％。
(2) 100g of copper smelting slag with granularity smaller than 0.075mm, which is crushed to be more than 90%, is added into an ultrasonic pressurizing reaction kettle, 600mL of NaOH solution with mass concentration of 25% is added, 10g of industrial sodium nitrate is added, and the mixture is reacted for 3.0h under mechanical stirring and ultrasonic irradiation at the temperature of 140 ℃; stopping heating after leaching, introducing cooling water to cool the solution to a temperature lower than 70deg.C, taking out ore pulp, performing solid-liquid separation, and washing the residue with 50mL of 80deg.C hot water for three times to obtain filtrate622mL, the filter residue is placed in an oven for drying at 120 ℃ for 2h, the weight of the filter residue is 65.5g, and Fe in the filter residue 2 O 3 The mass contents of Cu and S are 85.7%,0.30% and 0.20%, respectively, and can be directly used for ironmaking operation.
(3) 622mL of the obtained filtrate and washing liquid is heated to 80 ℃, 20% dilute sulfuric acid solution is added under stirring, the addition is carried out to adjust the pH of the solution to 3.0 as an end point, stirring is continued to react for 3.0h, stirring and aging are stopped for 2.5h, filtration is carried out, 50mL of deionized water is used for three times of washing, 50mL of absolute ethyl alcohol is used for three times of washing to obtain a filter cake, and the filter cake is dried in a drying oven at 110 ℃ for 2.0h to obtain 32.1g of white carbon black product. The oil absorption value of the prepared white carbon black product is 2.3mL/g, and the specific surface area reaches 296.60m 2 And/g, meets the national A-grade standard of white carbon black.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present application. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
While embodiments of the present application have been shown and described, it will be understood by those of ordinary skill in the art that: many changes, modifications, substitutions and variations may be made to the embodiments without departing from the spirit and principles of the application, the scope of which is defined by the claims and their equivalents.
Claims (4)
1. A method for separating silicon and iron in copper smelting slag by ultrasonic reinforcement and preparing white carbon black by utilizing silicon is characterized by comprising the following steps:
step 1, crushing: crushing copper smelting slag to obtain powdery copper smelting slag;
step 2, ultrasonic intensified leaching: adding 100g of the powdery copper smelting slag obtained in the step 1 into an ultrasonic pressurizing reaction kettle, adding 400-800 mL of sodium hydroxide solution with the mass concentration of 20-60%, adding sodium nitrate with the addition amount of 5-20% of the mass of the powdery copper smelting slag, stirring and reacting for 1.0-3.0 h at 120-200 ℃ under ultrasonic irradiation, and cooling the reactant to a temperature lower than 80 ℃ after the reaction is finished;
step 3, solid-liquid separation: carrying out solid-liquid separation and washing on the reactant cooled in the step 2 to obtain a filtering liquid and filter residues;
step 4, aging: heating the filtering and washing liquid obtained in the step 3 to 80-90 ℃, adding 10% -30% of dilute sulfuric acid solution under stirring to adjust the pH of the filtering and washing liquid to 2.5-3.5, continuously stirring and reacting for 1.0-2.0 h, and standing and ageing for 1.5-2.5 h after the reaction is finished to obtain an aged precipitate;
step 5, filtering: filtering and washing the precipitate obtained in the step 4 to obtain a filter cake;
step 6, drying: drying the filter cake obtained in the step 5 at 105-110 ℃ for 1-2 hours to obtain white carbon black;
the copper smelting slag comprises the following components in percentage by mass: fe 30% -50% and SiO 2 25%~35%、CaO 1.0%~10.0%、MgO 1.0%~5.0%、 Al 2 O 3 0.5%~5.0%、 Cu 0.1%~1.0%、 S 0.05%~1.0%。
2. The method for ultrasonic-enhanced separation of silicon and iron from copper smelting slag and preparation of white carbon black by utilizing silicon according to claim 1, wherein the method comprises the following steps: the granularity of the crushed powdery copper smelting slag in the step 1 is smaller than 0.075 and mm.
3. The method for ultrasonic-enhanced separation of silicon and iron from copper smelting slag and preparation of white carbon black by utilizing silicon according to claim 1, wherein the method comprises the following steps: the main component of the filter residue in the step 3 is hematite, which is a high-quality iron-making raw material for iron-making operation.
4. The method for ultrasonic-enhanced separation of silicon and iron from copper smelting slag and preparation of white carbon black by utilizing silicon according to claim 1, wherein the method comprises the following steps: and in the filtering step 5, the aged precipitate is filtered, and is washed three times by 50mL deionized water and is washed three times by 50mL absolute ethyl alcohol to obtain the filter cake.
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