CN115043471A - Method for preparing polysilicate aluminum ferric sulfate flocculant by using copper smelting furnace slag - Google Patents
Method for preparing polysilicate aluminum ferric sulfate flocculant by using copper smelting furnace slag Download PDFInfo
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- CN115043471A CN115043471A CN202210681595.6A CN202210681595A CN115043471A CN 115043471 A CN115043471 A CN 115043471A CN 202210681595 A CN202210681595 A CN 202210681595A CN 115043471 A CN115043471 A CN 115043471A
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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Abstract
The invention discloses a method for preparing a polysilicate ferric aluminum sulfate flocculating agent by using copper smelting furnace slag, which relates to the field of comprehensive utilization of copper smelting furnace slag resources and solves the problems of high difficulty and high cost of valuable metal recovery by existing mineral separation flotation; standing and precipitating the turbid stock solution at 50-70 ℃, and transferring a supernatant a after precipitation; adding hydrogen peroxide into the supernatant a, stirring and activating to obtain a supernatant b, adding aluminum hydroxide into the supernatant b, and adjusting the pH value to be less than 3 by using sulfuric acid after the reaction is finished; adjusting the pH value to be below 3 by using sulfuric acid, then aging, and drying to obtain a finished product of the polysilicate ferric sulfate aluminum flocculant; the method utilizes the slag, and the copper smelting system produces the sulfuric acid, so that the method can be used for acid washing, acid leaching and dissolving of the slag, is self-produced and self-sold, has low cost, produces valuable new products, has simple production process, and reduces the treatment difficulty and the treatment capacity of downstream mineral separation and flotation.
Description
Technical Field
The invention relates to the technical field of comprehensive utilization of copper smelting furnace slag resources, in particular to the technical field of preparation of a polysilicate aluminum ferric sulfate flocculant by using copper smelting furnace slag.
Background
Copper, located in group IB of the fourth stage of the periodic table of elements, is the first metal used by humans. Copper has excellent performance, is easy to process and has wide application, is widely applied to the fields of electricity, light industry, mechanical manufacturing, building industry, national defense industry and the like, and is second to aluminum in the consumption of nonferrous metal materials in China.
The pyrometallurgical copper smelting is the main method for producing copper at present, and copper ore is subjected to mining and mineral separation to obtain copper concentrate with high copper-containing grade, and then the copper concentrate is sent to a smelting plant for copper smelting. The pyrometallurgical copper smelting process flow generally comprises the steps of smelting matte to obtain matte; converting in a converter to obtain crude copper; refining by fire method to obtain anode copper; and (4) performing electrolytic refining to obtain cathode copper. Pyrometallurgical copper smelting produces large quantities of slag per day, roughly two tons of slag per ton of copper produced, where large quantities of the iron silicon element are not utilized efficiently. Beneficiation and flotation are the main copper smelting slag treatment methods at present, and slag concentrate and tailings are obtained, wherein the slag concentrate is returned to a furnace for valuable metal recovery, and the tailings are subjected to other treatments.
Application number CN201510042614.0 discloses a process method suitable for simultaneously sorting copper smelting electric furnace slag and converter slag, which comprises the following steps: if the raw ore is electric furnace slag, entering two-stage continuous ore grinding-flotation process, and if the raw ore is converter slag, entering two-stage ore grinding-two-stage flotation process; the invention has the advantages that the optimal process flow for selecting the electric furnace slag and the converter slag is respectively researched and provided; the screening index of 0.188 of copper content in tailings is obtained by adopting the combined medicine of water glass, sodium bicarbonate and sodium sulfide in the screening of converter slag. The invention can adjust connection according to ore types, and satisfies the continuous ore grinding-flotation process of two sections of electric furnace slag and the continuous ore grinding-flotation process of two sections of converter slag, and the recovery rate of copper in the obtained copper concentrate is less than 80%.
The problem that above-mentioned patent exists is that the technology of ore dressing flotation recovery valuable metal is complicated, and the degree of difficulty is high, and the cost is also high.
Disclosure of Invention
The invention aims to: in order to solve the technical problems of high difficulty and high cost of recovering valuable metals by the conventional beneficiation and flotation, the invention provides a method for preparing a polysilicate ferric aluminum sulfate flocculating agent by using copper smelting furnace slag.
The invention specifically adopts the following technical scheme for realizing the purpose: the method for preparing the polysilicate aluminum ferric sulfate flocculant by using the copper smelting furnace slag comprises the following steps:
step 2, standing the turbid stock solution for 2-4 hours at 50-70 ℃ for precipitation, and transferring supernatant a after precipitation;
step 3, adding hydrogen peroxide into the supernatant a, stirring and activating to obtain a supernatant b, adding aluminum hydroxide into the supernatant b, and adjusting the pH value to be less than 3 by using sulfuric acid after the reaction is finished;
and 4, adjusting the pH value to be below 3 by using sulfuric acid, then aging, washing with water, filtering to obtain a semi-finished product of the polysilicate aluminum ferric sulfate flocculant, and drying to obtain a finished product of the polysilicate aluminum ferric sulfate flocculant.
According to the technical scheme, the characteristics that the furnace slag contains high-iron and high-silicon dioxide are utilized, the furnace slag contains 25-45% of iron and 20-40% of silicon dioxide, sulfuric acid recovered and produced by sulfur dioxide in copper smelting flue gas, namely sulfuric acid produced by the self-production is subjected to acid pickling, acid leaching, dissolving and activating, then precipitation is carried out, clear liquid after precipitation is added with hydrogen peroxide and aluminum hydroxide for stirring, and the mixture is kept stand and aged for enough time after complete reaction, so that the ferric aluminum silicate sulfate flocculant can be obtained. The precipitated precipitate can be sent to mineral separation flotation after being dried/air-dried at low temperature, and is used as a raw material for producing slag concentrate for recycling valuable metals. The method has the advantages that the furnace slag is utilized, meanwhile, the copper smelting system produces sulfuric acid by itself, the sulfuric acid can be used for acid pickling, acid pickling and dissolving of the furnace slag, the product is produced by itself, the product of the system is fully utilized, the production cost has great advantages, the furnace slag is comprehensively utilized to produce the polysilicate ferric aluminum sulfate flocculating agent, the valuable new product is produced, the production process is simple and is a wet method, smoke and waste liquid and waste residues are avoided, all products are not produced additionally in a closed circuit mode, the total amount of the furnace slag is reduced, the energy waste in the material transportation process is reduced, the pollution and the influence of the material scattering on the surrounding environment are reduced, and the treatment difficulty and the treatment capacity of downstream (valuable metal recovery) flotation ore dressing are reduced.
Further, in the step 1, 1-1.5 t of slag is added into 1.8-2.5 t of 30% sulfuric acid solution.
Further, in the step 3, 500-600 kg of hydrogen peroxide (1.2-1.5 times of excess hydrogen peroxide can be added to each ton of supernatant a, and the reaction speed is higher).
Further, the stirring and activating time in the step 3 is 1-2 hours.
Further, 200-300 kg of aluminum hydroxide (preferably 120-200 mg/L of aluminum ion concentration) is added to each ton of supernatant b.
Further, the aging time in the step 4 is 8-10 hours, and the drying temperature is 90-110 ℃.
Further, the sulfuric acid solution is obtained by the following method: after smelting raw material copper concentrate (containing 20-30% of sulfur) is reacted and combusted in a smelting furnace (most of sulfur reacts with oxygen in industrial air at the temperature of over 1100 ℃ to generate sulfur dioxide), flue gas (the flue gas is mixed with a large amount of smoke dust, cannot be randomly discharged, or seriously pollutes the environment) enters an acid making system after being dedusted and cooled by a waste heat boiler and an electric dust collector, and is purified, dry absorbed and converted by the acid making system to prepare sulfuric acid solution.
Further, the precipitate in the step 2 is stirred and dried at 95-105 ℃ (sent to beneficiation and flotation) to be used as a raw material for producing slag concentrate, and valuable metals (including copper, gold and silver) are recovered.
The invention has the following beneficial effects:
1. comprehensive utilization of resources: the method comprises the following steps of (1) utilizing high-concentration iron and silicon dioxide in slag, wherein the slag contains 25-45% of iron and 20-40% of silicon dioxide, and generating about 2-3 tons of slag every time a copper smelting system produces one ton of copper, and taking a copper smelting system with 20 ten thousand tons of energy production as an example, generating about 50 ten thousand tons of slag every year; meanwhile, sulfuric acid produced by recovering sulfur dioxide in copper smelting flue gas is utilized, and about 75 ten thousand tons of sulfuric acid (equivalent to 100% sulfuric acid) is produced every year by taking a copper smelting system with 20 ten thousand tons of energy production as an example, so that the raw materials are sufficient;
2. the production cost is reduced: the slag is utilized, and meanwhile, the copper smelting system produces sulfuric acid, so that the sulfuric acid can be used for acid pickling, acid leaching and dissolving of the slag, is self-produced and self-sold, fully utilizes the products of the system, and has great advantage in production cost;
3. the total amount of the slag is reduced: the slag is comprehensively utilized to produce the polysilicate aluminum ferric sulfate flocculant, the total amount of the slag is estimated to be reduced by about 1/4-1/3, and the environmental pollution is reduced. The treatment difficulty and treatment capacity of downstream beneficiation and flotation are reduced;
4. environmental protection benefit: the production process is simple and is a wet method, no smoke, waste liquid and waste residues exist, and all products are closed without extra output. Meanwhile, the total amount of the furnace slag is reduced, the energy waste in the material transporting process is reduced, and the pollution and influence of the material scattering on the surrounding environment are reduced, so that the method has certain social and environmental benefits;
5. economic benefits are as follows: the produced polysilicate aluminum ferric sulfate is a high-efficiency water purification flocculant, has low economic value and has great significance for comprehensive utilization of resources.
Drawings
FIG. 1 is a flow chart of the method for preparing a polysilicate aluminum ferric sulfate flocculant from copper smelting slag according to the present invention;
FIG. 2 is a graph of a sample of the polyaluminum ferric silicate sulfate flocculant produced in example 2;
FIG. 3 is an XRD diffraction pattern of the polysilicate aluminum ferric sulfate flocculant produced in example 2;
FIG. 4 is a Fourier infrared spectrum of the aluminum ferric polysilicate sulfate flocculant produced in example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments.
Therefore, all other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative effort belong to the protection scope of the present invention.
Example 1
As shown in fig. 1, this example provides a method for preparing polysilicate aluminum ferric sulfate flocculant from copper smelting slag, which comprises the following steps:
preparing a sulfuric acid solution: because the smelting raw material copper concentrate contains about 20-30% of sulfur, most of the sulfur reacts with oxygen in industrial air at the temperature of over 1100 ℃ to generate sulfur dioxide after the smelting furnace reacts and burns, and smoke gas is mixed with a large amount of smoke dust which cannot be discharged randomly, otherwise, the environment is seriously polluted. After being dedusted and cooled by a waste heat boiler and an electric dust collector, the waste heat boiler and the electric dust collector enter an acid making system to be used for producing sulfuric acid. The concentrated sulfuric acid with high purity is prepared by three main processes of purification, dry absorption and conversion of an acid making system, and is diluted to about 30% for preparing the polysilicate ferric aluminum sulfate flocculant.
step 2, standing the turbid stock solution for 2 hours at 50 ℃ for precipitation, and transferring supernatant a after precipitation; stirring and drying the precipitate at 95 ℃ (sending the precipitate to mineral separation and flotation) to be used as a raw material for producing slag concentrate, and recovering valuable metals (the valuable metals comprise copper, gold and silver);
step 3, adding hydrogen peroxide into the supernatant a, adding 500kg of hydrogen peroxide into each ton of the supernatant a, stirring and activating for 1 hour to obtain a supernatant b, adding aluminum hydroxide into the supernatant b, adding 200kg of aluminum hydroxide into each ton of the supernatant b, and adjusting the pH value to be less than 3 by using sulfuric acid after the reaction is finished;
and 4, adjusting the pH value to be below 3 by using sulfuric acid, aging for 8 hours, washing and filtering to obtain a semi-finished product of the polysilicate aluminum ferric sulfate flocculant, and drying to obtain a finished product of the polysilicate aluminum ferric sulfate flocculant, wherein the drying temperature is 90 ℃.
Example 2
As shown in fig. 1-4, step 1, adding 1.2t of slag into 2.2t of 30% sulfuric acid solution, stirring and washing at 60 ℃ until the dissolution is completed to obtain turbid stock solution;
step 2, standing the turbid stock solution for 3 hours at the temperature of 60 ℃ for precipitation, and transferring supernatant a after precipitation; stirring and drying the precipitate at 100 ℃ (sending the precipitate to mineral separation and flotation) to be used as a raw material for producing slag concentrate, and recovering valuable metals (the valuable metals comprise copper, gold and silver);
step 3, adding hydrogen peroxide into the supernatant a, adding 550kg of hydrogen peroxide into each ton of the supernatant a, stirring and activating for 1.5 hours to obtain a supernatant b, adding aluminum hydroxide into the supernatant b, adding 250kg of aluminum hydroxide into each ton of the supernatant b, and adjusting the pH to be less than 3 by using sulfuric acid after the reaction is finished;
and 4, adjusting the pH value to be below 3 by using sulfuric acid, aging for 9 hours, washing with water, filtering to obtain a semi-finished product of the polysilicate aluminum ferric sulfate flocculant, and drying to obtain a finished product of the polysilicate aluminum ferric sulfate flocculant, wherein the drying temperature is 100 ℃. Wherein the sulfuric acid is prepared as described in example 1.
The finished product of the polysilicate aluminum ferric sulfate flocculant prepared in the embodiment is analyzed by an XRD diffractometer to obtain a characteristic spectrogram as shown in figure 3, and the diffraction peak is mainly ferric sulfate and has low intensity, which indicates that partial polymerization occurs; no peak was observed for aluminum sulfate, indicating that this part of the polymerization was relatively complete.
The polysilicate aluminum ferric sulfate flocculant finished product prepared in the embodiment is analyzed by a Fourier infrared spectrometer to obtain a spectrogram shown in figure 4, and 3400-3500 cm can be observed -1 The wide absorption peak in the range is the stretching vibration absorption peak of Si-OH, and is 1600-1700 cm -1 Absorption peak in the range of H in the sample which is not completely dried 2 O，1000～1150cm -1 The nearby absorption peak is the stretching vibration absorption peak of Si-O-Si, and is 500-650 cm -1 The nearby absorption peak is the absorption peak of O-Si-O, and the sulfuric acid participates in the activation process, and is 900-1000 cm -1 The nearby peak is the absorption peak of sulfate radical, and is partially overlapped with the large absorption peak to cause less obvious, and 700-800 cm -1 The two nearby peaks that are relatively close are the vibrational peaks of Fe-O-Si and Al-O-Si. It can be judged that the sample is based on polysilicic acid, and is combined with a high molecular polymer of iron and aluminum, and the obtained product is polysilicic acid ferric aluminum sulfate.
Example 3
As shown in fig. 1, step 1, adding 1.5t of slag into 2.5t of 30% sulfuric acid solution, stirring and washing at 70 ℃ until the dissolution is completed to obtain turbid stock solution;
step 2, standing the turbid stock solution for 4 hours at 70 ℃ for precipitation, and transferring supernatant a after precipitation; stirring and drying the precipitate at 105 ℃ (sending the precipitate to beneficiation and flotation) to be used as a raw material for producing slag concentrate, and recovering valuable metals (the valuable metals comprise copper, gold and silver);
step 3, adding hydrogen peroxide into the supernatant a, adding 600kg of hydrogen peroxide into each ton of the supernatant a, stirring and activating for 2 hours to obtain a supernatant b, adding aluminum hydroxide into the supernatant b, adding 300kg of aluminum hydroxide into each ton of the supernatant b, and adjusting the pH to be less than 3 by using sulfuric acid after the reaction is finished;
and 4, adjusting the pH value to be below 3 by using sulfuric acid, then aging for 10 hours, washing with water, filtering to obtain a semi-finished product of the polysilicate aluminum ferric sulfate flocculant, and drying to obtain a finished product of the polysilicate aluminum ferric sulfate flocculant, wherein the drying temperature is 110 ℃. Wherein the sulfuric acid is prepared as described in example 1.
Example 4
Application example:
step 2, keeping the water bath kettle at the constant temperature of 70 ℃, standing for 4 hours for precipitation, performing suction filtration by using a Buchner funnel and medium-speed filter paper to obtain a clarified liquid a, weighing 395g and about 280 mL; putting the filtered precipitate into an oven at 105 +/-5 ℃ for drying for 2 hours to obtain precipitate, and weighing 146g of the precipitate;
step 3, adding 240g of hydrogen peroxide (30%) into the clarified liquid a, stirring by using an automatic stirrer, activating for 1.5h, adding 160g of aluminum hydroxide (AR analytically pure), continuously stirring until the reaction is finished, and adjusting the pH to 2.9 by using 30% sulfuric acid to obtain a turbid liquid with the volume of about 890 mL;
and 4, aging the turbid solution for 8.5h, performing suction filtration by using a Buchner funnel and medium-speed filter paper, washing by using about 10mL of water while filtering, putting the filtered precipitate into an oven, drying for 2h at 105 +/-5 ℃, and weighing to obtain 92g of pale yellow powdery solid, namely the finished product of the polysilicate ferric aluminum sulfate flocculant.
Step 5, taking 500mL of concentrate dust washing wastewater (containing 28.32g of insoluble concentrate dust) of an open-air emergency pool into a 1000mL beaker, adding 10g of the polysilicate aluminum ferric sulfate prepared in the step 4 into the beaker, slightly stirring uniformly, and standing for about 25 minutes;
and 6, clarifying the upper part of the solution, wherein the lower half part of the solution contains the copper concentrate powder floccule with deep color, and detecting the removal rate of insoluble copper concentrate powder to be 98.03 percent.
Claims (8)
1. The method for preparing the polysilicate aluminum ferric sulfate flocculating agent by using the copper smelting slag is characterized by comprising the following steps of:
step 1, adding furnace slag into a sulfuric acid solution, stirring and washing at 50-70 ℃ until dissolution is completed to obtain a turbid stock solution;
step 2, standing the turbid stock solution for 2-4 hours at 50-70 ℃ for precipitation, and transferring supernatant a after precipitation;
step 3, adding hydrogen peroxide into the supernatant a, stirring and activating to obtain a supernatant b, adding aluminum hydroxide into the supernatant b, and adjusting the pH value to be less than 3 by using sulfuric acid after the reaction is finished;
and 4, adjusting the pH value to be below 3 by using sulfuric acid, then aging, washing with water, filtering to obtain a semi-finished product of the polysilicate aluminum ferric sulfate flocculant, and drying to obtain a finished product of the polysilicate aluminum ferric sulfate flocculant.
2. The method for preparing the polysilicate aluminum ferric sulfate flocculant from the copper smelting slag according to claim 1, wherein 1-1.5 t of the slag is added to 1.8-2.5 t of 30% sulfuric acid solution in the step 1.
3. The method for preparing the polysilicate aluminum ferric sulfate flocculant by using the copper smelting slag according to the claim 1, wherein 500-600 kg of hydrogen peroxide is added into each ton of supernatant a in the step 3.
4. The method for preparing the polysilicate aluminum ferric sulfate flocculant by using the copper smelting slag according to the claim 1, wherein the stirring and activating time in the step 3 is 1-2 hours.
5. The method for preparing the polysilicate aluminum ferric sulfate flocculant by using the copper smelting slag according to claim 1, wherein 200-300 kg of aluminum hydroxide is added to each ton of supernatant b.
6. The method for preparing the polysilicate aluminum ferric sulfate flocculating agent by using the copper smelting slag according to the claim 1, wherein the aging time in the step 4 is 8-10 hours, and the drying temperature is 90-110 ℃.
7. The method for preparing the polysilicate aluminum ferric sulfate flocculant from the copper smelting slag according to the claim 1 or 2, wherein the sulfuric acid solution is obtained by the following method: after smelting raw material copper concentrate is reacted and combusted in a smelting furnace, smoke enters an acid making system after being dedusted and cooled by a waste heat boiler and an electric dust collector, and is purified, dry absorbed and converted by the acid making system to prepare sulfuric acid solution.
8. The method for preparing the polysilicate aluminum ferric sulfate flocculant from the copper smelting slag according to claim 1, wherein the precipitate obtained in the step 2 is stirred and dried at 95-105 ℃ to be used as a raw material for producing slag concentrate, and valuable metals are recovered, wherein the valuable metals comprise copper, gold and silver.
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Cited By (1)
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| CN117069232A (en) * | 2023-10-17 | 2023-11-17 | 中国科学院过程工程研究所 | Resource utilization method of chromium-containing gasification slag impurity removal acid liquor |
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