High-antimony lead production process based on lead refining alkaline residues
Through the porous anthracite process modified by urea intercalculation and nano-calcium oxide, the problems of low alkali utilization and low recovery efficiency in traditional lead smelting processes are solved, and efficient production and economic benefits of high antimony lead are achieved.
Patent Information
- Application Number
- CN202510453529.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-11
- Publication Date
- 2025-06-13
AI Technical Summary
In the traditional low-temperature alkaline lead smelting process, the effective utilization rate of alkali is low, resulting in low lead recovery efficiency and antimony recovery efficiency. At the same time, the amount of slag produced is large and the lead content in the slag is high, which affects economic benefits.
The urea intercalation is followed by carbonization to form porous anthracite, and the porous anthracite is modified through the second intercalation of nano calcium oxide, which significantly improves the reaction activity and pore structure and improves the efficiency of anthracite reduction reaction. The process is melted in a vacuum furnace, and high antimony lead is prepared using modified porous anthracite, iron filings and copper powder.
It improves the purity of lead products and antimony recycling efficiency, reduces the amount of slag and the content of lead in the slag, reduces the loss of lead, and significantly improves economic benefits.
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Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of crude lead refining alkali slag, and particularly relates to a high-antimony lead production process based on lead refining alkali slag. Background Art
[0002] Due to the low melting point, high volatility and high toxicity of lead, the most promising smelting process is the low-temperature pyrometallurgical process. The traditional low-temperature alkali method for lead smelting is as follows: NaOH is mixed with raw materials at a weight ratio of 0.7 - 1.0, added to the furnace and smelted at 600 - 700 °C. More than 97% of the lead in the concentrate can be recovered, and 97 - 98% of the precious copper powder is enriched in the lead. Copper, zinc, etc. in the raw materials have basically no influence on the smelting process. Sulfur and other components enter the alkaline dross. Sodium hydroxide may react with various copper powder oxides and sulfides, resulting in partial consumption of the alkali in non-target reactions, reducing the effective utilization rate of the alkali. The main reaction of this process is that only one-third of the NaOH in the batching participates in the above reaction, and the rest is used to maintain the fluidity of the molten dross at the smelting temperature.
[0003] Chinese Patent Publication No. CN108220624B discloses a method for treating crude lead refining alkali slag. The method is to crush and grind the tin-containing lead alkali slag (crude lead refining alkali slag), mix the obtained ore powder with sodium hydroxide to form a slurry, and then carry out leaching under normal pressure, liquid-solid separation to obtain a tin-containing leaching solution and a lead-containing leaching residue; the tin-containing leaching solution is causticized with calcium oxide to obtain calcium stannate precipitate and causticized solution; the obtained calcium stannate is subjected to reduction smelting with a carbonaceous reducing agent to obtain crude tin and calcium oxide. However, in this scheme, calcium oxide causticizes the sodium stannate solution to convert sodium stannate into insoluble calcium stannate precipitate, making it easy to separate calcium stannate from the solution system. Calcium oxide is prone to agglomeration during the causticization process of the tin-containing leaching solution, reducing the causticization efficiency of calcium oxide for the sodium stannate solution, and thus affecting the recovery rate of the product. Summary of the Invention
[0004] The purpose of the present invention is to provide a high-antimony lead production process based on lead refining alkali slag. After urea intercalation and carbonization treatment, urea decomposes and escapes, leaving more pores and larger interlayer spacing, which increases the specific surface area of anthracite to obtain porous anthracite. Nano calcium oxide is used for the second intercalation of the porous anthracite to obtain modified porous anthracite with larger interlayer spacing, larger surface area, and a large amount of nano calcium oxide evenly attached to the surface, significantly improving the reaction activity. The increased pore structure helps the diffusion of gas, thereby improving the efficiency of the anthracite reduction reaction; the lead product prepared by this production process has high purity, high antimony recovery efficiency, and at the same time produces less slag and the lead content in the slag is low.
[0005] The purpose of the present invention can be achieved by the following technical solutions: A high-antimony lead production process based on lead-refining alkali slag is prepared through the following steps: Step 1: Add urea and deionized water into a reaction kettle, stir at 20 - 25°C and 400 - 500 r / min for 30 - 40 min. Crush anthracite to 1 - 2 mm, dry it at 105 - 120°C for 2 - 3 h, mix it with sodium dodecyl sulfate and add it into the reaction kettle. Under the conditions of 50 - 65°C and 400 - 500 r / min, carry out vacuum impregnation for 2 - 3 h. Filter, wash the filter cake with deionized water and absolute ethanol respectively for 2 - 3 times to remove the residual urea solution on the surface. Vacuum dry at 60 - 80°C for 1 - 2 h, grind, sieve through a 100 - 120 mesh sieve, transfer it to a muffle furnace, keep it warm at 800 - 900°C under nitrogen protection for 4 - 6 h, and cool naturally to obtain porous anthracite.
[0006] Step 2: Add nano-calcium oxide with a particle size of 50 - 100 nm and deionized water into a reaction kettle, stir at 20 - 25°C and 400 - 500 r / min for 30 - 40 min, carry out ultrasonic dispersion for 30 - 40 min, add porous anthracite, and carry out vacuum impregnation at 50 - 65°C and a stirring rate of 400 - 500 r / min for 2 - 3 h. Cool naturally, stand for 24 - 26 h, filter, wash the filter cake with deionized water and absolute ethanol respectively for 2 - 3 times, and vacuum dry to obtain modified porous anthracite.
[0007] Step 3: Add asphalt powder with a particle size of 3 - 5 mm and sodium dodecyl sulfate into a reaction kettle, keep it warm at 135 - 140°C for 20 - 30 min, then add zeolite powder, stir at 400 - 500 r / min for 30 - 40 min, continue to stir and keep warm for 15 - 20 min, shear at a rate of 3000 - 4000 r / min for 1 - 2 h, grind, cool naturally, and sieve through an 80 - 100 mesh sieve to obtain zeolite-based modified asphalt powder; Add the modified porous anthracite and zeolite-based modified asphalt powder into the reaction kettle, stir at 135 - 140°C for 8 - 12 min, knead and process into spheres, transfer it to a muffle furnace, keep it warm at 800 - 900°C under nitrogen protection for 4 - 6 h, and cool naturally to obtain spherical modified porous anthracite with a particle size of 1 - 2 cm.
[0008] Step 4: Crush the lead alkali slag, screen it through a 100 - 120 mesh sieve, and slurry it with sodium hydroxide at a concentration of 80 - 85 g / L. Add the slurried material into the leaching tank, leach it at 80 - 85 °C for 2 - 3 h, then perform liquid - solid separation, and vacuum dry it at 60 - 80 °C for 1 - 2 h to obtain refined lead alkali slag. Transfer the refined lead alkali slag to a converter, use natural gas - oxygen as fuel, add modified porous anthracite, iron filings, and copper powder into the converter, melt it at 1100 - 1200 °C for 6 - 8 h, discharge the crude lead from the converter and slag. The crude lead from the converter enters a vacuum furnace after impurity removal, and under the conditions of a vacuum degree of 20 - 30 Pa, a power of 290 - 310 kW, and a gas flow rate of 12 - 14 kg / min, perform vacuum separation to collect high - antimony lead, thus completing a production process of high - antimony lead based on refined lead alkali slag.
[0009] Further, the dosage ratio of urea, deionized water, sodium dodecyl sulfate, and anthracite is 20 - 30 mL: 300 - 400 mL: 1 - 2 g: 30 - 40 g.
[0010] Further, the dosage ratio of nano - calcium oxide, deionized water, and porous anthracite is 20 - 30 g: 300 - 400 mL: 20 - 23 g.
[0011] Further, the dosage ratio of asphalt powder, sodium dodecyl sulfate, and zeolite is 20 - 23 g: 1 - 2 g: 4 - 5 g.
[0012] Further, the dosage ratio of modified porous anthracite and zeolite - based modified asphalt powder is 30 - 40 g: 4 - 5 g.
[0013] Further, the dosage ratio of lead alkali slag and sodium hydroxide is 400 - 500 g: 3 - 4 L.
[0014] Further, the dosage ratio of refined lead alkali slag, modified porous anthracite, iron filings, and copper powder is 30 - 40 g: 70 - 80 g: 50 - 60 g: 10 - 12 g.
[0015] Advantages of the present invention: 1. The production process of high - antimony lead prepared by the present invention is characterized in that the prepared lead product has high purity, high antimony recovery efficiency, less slag is generated at the same time, and the lead content in the slag is low, effectively reducing the loss of lead and significantly improving the economic benefits.
[0016] 2. The porous anthracite of the present invention is carbonized after urea intercalation. Urea decomposes and escapes, leaving more pores and larger interlayer spacing. This increases the specific surface area of anthracite, significantly improves the reaction activity, and the increased pore structure helps the diffusion of gas, thus improving the efficiency of the reduction reaction and removing some organic impurities. During the carbonization process, some organic impurities in anthracite will be decomposed or volatilized, thus reducing the interference of impurities on the reduction reaction.
[0017] 3. Sulfides in anthracite are prone to volatilize at high temperatures and enter the gas phase, resulting in environmental pollution and equipment corrosion. Nano-calcium oxide is intercalated on the surface and inside the modified porous anthracite of the present invention, which can react with sulfides to form stable calcium sulfate, thereby fixing sulfides and reducing their volatilization. Calcium oxide can also react with acidic oxides in ash to form stable compounds, thereby reducing the negative impact of ash on the reduction reaction. The increased pore structure and layer spacing increase the contact area between anthracite and the reaction system, resulting in a faster reaction rate and higher reduction efficiency.
[0018] 4. The present invention uses zeolite-based modified asphalt powder as a binder for modified porous anthracite. Zeolite has high porosity and high specific surface area, which enables zeolite particles to form more contact points and bonding surfaces in asphalt. These contact points and bonding surfaces increase the interaction force between asphalt and anthracite, thereby improving the bonding strength. Zeolite particles can fill the microscopic pores and cracks in asphalt, reduce the void ratio, and improve the density of asphalt. This filling effect makes the contact between asphalt and aggregate closer, thereby improving the bonding strength and helping to form a stronger coal ball, reducing the emission of harmful substances such as soot and harmful gases, and thus reducing environmental pollution. Specific Embodiments
[0019] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.
[0020] Example 1: A high-antimony lead production process based on lead-refining alkali slag is prepared through the following steps: S1: Add 20 mL of urea and 300 mL of deionized water to a reaction kettle, stir at 20 °C and 400 r / min for 30 min. Crush 30 g of anthracite to 1 - 2 mm, dry it at 105 °C for 2 h, mix it with 1 g of surfactant sodium dodecyl sulfate, add it to the reaction kettle, and vacuum impregnate it at 50 °C and 400 r / min for 2 h. Filter, wash the filter cake twice with deionized water and anhydrous ethanol respectively to remove the residual urea solution on the surface, vacuum dry it at 60 °C for 1 h, grind it, pass it through a 100-mesh sieve, transfer it to a muffle furnace, and keep it at 800 °C for 4 h under nitrogen protection, and then cool it naturally to obtain porous anthracite.
[0021] The amino group and carbonyl group in the urea molecule can form hydrogen bonds with functional groups such as hydroxyl groups and carboxyl groups on the surface or inside of anthracite, thereby adsorbing on the surface of anthracite or entering its interior; urea decomposes urea by pyrolysis to release ammonia, and the ammonia is used to react with the hard components on the material surface.
[0022] S2: Add 20 g of nano-calcium oxide with a particle size of 50 - 100 nm and 300 mL of deionized water to the reaction kettle, stir for 30 min at 20 °C and 400 r / min, ultrasonically disperse for 30 min, add 20 g of porous anthracite to the reaction kettle, and carry out vacuum impregnation at 50 °C and 400 r / min for 2 h, then cool naturally and stand for 24 h to allow the nano-calcium oxide to fully penetrate into the pores of the coal. Filter, wash the filter cake twice with deionized water and anhydrous ethanol respectively to remove the residual nano-calcium oxide suspension on the surface, and dry in vacuum at 60 °C for 1 h to obtain modified porous anthracite.
[0023] S3: Add 20 g of asphalt powder with a particle size of 3 - 5 mm and 1 g of sodium dodecyl sulfate as a surfactant to the reaction kettle, keep warm at 135 °C for 20 min, then add 4 g of zeolite powder, stir at 400 r / min for 30 min, continue stirring and keeping warm for 15 min, shear at a rate of 3000 r / min for 1 - 2 h, grind, cool naturally, and pass through an 80-mesh sieve to obtain zeolite-based modified asphalt powder; add 30 g of modified porous anthracite and 4 g of zeolite-based modified asphalt powder to the reaction kettle, stir at 135 °C for 8 - 12 min, knead and process into spheres, transfer to a muffle furnace, and keep warm at 800 °C under nitrogen protection for 4 h, then cool naturally to obtain spherical modified porous anthracite with a particle size of 1 - 2 cm.
[0024] After surface modification of the asphalt powder and compounding with zeolite, zeolite-based modified asphalt powder is obtained. Zeolite has high porosity and high specific surface area, which enables zeolite particles to form more contact points and bonding surfaces in the asphalt. These contact points and bonding surfaces increase the interaction force between the asphalt and anthracite, thereby improving the bonding strength. S4: Crush 400 g of lead alkaline slag, pass through a 100-mesh sieve, and adjust the slurry with 3 L of sodium hydroxide with a concentration of 80 g / L. Add the adjusted material to the leaching tank, carry out liquid-solid separation after leaching at 80 °C for 2 h, and dry in vacuum at 60 - 80 °C for 1 - 2 h to obtain refined lead alkaline slag; transfer 30 g of refined lead alkaline slag to the converter, use natural gas-oxygen as fuel, add 70 g of modified porous anthracite, 50 g of iron filings and 10 g of copper powder to the converter, melt at 1100 °C for 6 h, discharge the crude lead from the converter and slag. The crude lead from the converter is decontaminated through the decontamination process and then enters the vacuum furnace. Vacuum separation is carried out under the conditions of a vacuum degree of 20 Pa, a power of 290 kW, and a gas flow rate of 12 kg / min to obtain a high-antimony lead based on refined lead alkaline slag.
[0025] Example 2: A high-antimony lead production process based on lead-refining alkali slag is prepared through the following steps: S1: Add 25 mL of urea and 350 mL of deionized water into a reaction kettle, stir for 35 min at 23°C and 450 r / min, crush 35 g of anthracite to 1 - 2 mm, dry it at 110°C for 2.3 h, mix it with 1.2 g of sodium dodecyl sulfate as a surfactant and add it into the reaction kettle, carry out vacuum impregnation for 2 h at 60°C and 450 r / min, filter, wash the filter cake twice with deionized water and absolute ethanol respectively to remove the residual urea solution on the surface, vacuum dry at 70°C for 1.2 h, grind, sieve through a 110-mesh sieve, transfer it to a muffle furnace, keep it warm at 820°C for 4.6 h under nitrogen protection, and cool naturally to obtain porous anthracite.
[0026] S2: Add 25 g of nano-calcium oxide with a particle size of 50 - 100 nm and 350 mL of deionized water into a reaction kettle, stir for 35 min at 23°C and 450 r / min, carry out ultrasonic dispersion for 35 min, add 22 g of porous anthracite into the reaction kettle, carry out vacuum impregnation for 2.3 h at 60°C and 450 r / min, cool naturally, stand for 25 h to allow the nano-calcium oxide to fully penetrate into the pores of the coal, filter, wash the filter cake twice with deionized water and absolute ethanol respectively to remove the residual nano-calcium oxide suspension on the surface, vacuum dry at 70°C for 1.2 h to obtain modified porous anthracite.
[0027] S3: Add 21 g of asphalt powder with a particle size of 3 - 5 mm and 1.2 g of sodium dodecyl sulfate as a surfactant into a reaction kettle, keep it warm at 138°C for 25 min, then add 4.5 g of zeolite powder, stir at 450 r / min for 35 min, continue stirring and keep it warm for 18 min, shear at a rate of 3500 r / min for 1.2 h, grind, cool naturally, sieve through a 90-mesh sieve to obtain zeolite-based modified asphalt powder; add 35 g of modified porous anthracite and 4.5 g of zeolite-based modified asphalt powder into a reaction kettle, stir at 138°C for 10 min, knead and process it into a sphere, transfer it to a muffle furnace, keep it warm at 850°C for 4.6 h under nitrogen protection, and cool naturally to obtain spherical modified porous anthracite with a particle size of 1 - 2 cm.
[0028] S4: Crush 450 g of lead alkali slag, sieve it through a 110-mesh sieve, and slurry it with 3.4 L of sodium hydroxide with a concentration of 83 g / L. Add the slurried material into the leaching tank, leach it at 83 °C for 2.3 h, then perform liquid-solid separation, and vacuum dry it at 60 - 80 °C for 1 - 2 h to obtain refined lead alkali slag. Transfer 35 g of refined lead alkali slag to a converter, use natural gas-oxygen as fuel, add 75 g of modified porous anthracite, 55 g of iron filings, and 11 g of copper powder into the converter, melt it at 1150 °C for 7 h, discharge the crude lead from the converter and slag. After the crude lead from the converter is decontaminated through the decontamination process, it enters a vacuum furnace, and under the conditions of a vacuum degree of 25 Pa, a power of 300 kW, and a gas flow rate of 13 kg / min, perform vacuum separation to obtain a high-antimony lead based on refined lead alkali slag.
[0029] Example 3: A production process of high-antimony lead based on refined lead alkali slag is prepared through the following steps: S1: Add 30 mL of urea and 400 mL of deionized water into a reaction kettle, stir at 25 °C and 500 r / min for 40 min. Crush 40 g of anthracite to 1 - 2 mm, dry it at 120 °C for 3 h, mix it with 2 g of surfactant sodium dodecyl sulfate and add it into the reaction kettle, perform vacuum impregnation at 65 °C and 500 r / min for 3 h, filter, wash the filter cake 3 times with deionized water and anhydrous ethanol respectively to remove the residual urea solution on the surface, vacuum dry it at 80 °C for 2 h, grind it, sieve it through a 120-mesh sieve, transfer it to a muffle furnace, keep it at 900 °C for 6 h under nitrogen protection, and cool it naturally to obtain porous anthracite.
[0030] S2: Add 30 g of nano-calcium oxide with a particle size of 50 - 100 nm and 400 mL of deionized water into a reaction kettle, stir at 25 °C and 500 r / min for 40 min, ultrasonically disperse for 40 min, add 23 g of porous anthracite into the reaction kettle, perform vacuum impregnation at 65 °C and 500 r / min for 3 h, cool it naturally, and let it stand for 26 h to allow the nano-calcium oxide to fully penetrate into the pores of the coal. Filter, wash the filter cake 3 times with deionized water and anhydrous ethanol respectively to remove the residual nano-calcium oxide suspension on the surface, vacuum dry it at 80 °C for 2 h to obtain modified porous anthracite.
[0031] S3: Add 23 g of asphalt powder with a particle size of 3 - 5 mm and 2 g of sodium dodecyl sulfate as a surfactant into the reaction kettle, keep it at 140 °C for 30 min, then add 5 g of zeolite powder, stir at 500 r / min for 40 min, continue stirring and keep warm for 20 min, shear at a rate of 4000 r / min for 2 h, grind, cool naturally, and pass through a 100 - mesh sieve to obtain zeolite - based modified asphalt powder; Add 40 g of modified porous anthracite and 5 g of zeolite - based modified asphalt powder into the reaction kettle, stir at 140 °C for 12 min, knead and process into spheres, transfer to a muffle furnace, keep warm at 900 °C under nitrogen protection for 6 h, and cool naturally to obtain spherical modified porous anthracite with a particle size of 1 - 2 cm.
[0032] S4: Crush 500 g of lead - containing alkali slag, pass through a 120 - mesh sieve, and slurry it with 4 L of sodium hydroxide with a concentration of 85 g / L. Add the slurried material into the leaching tank, leach at 85 °C for 3 h and then perform liquid - solid separation, and vacuum - dry at 60 - 80 °C for 1 - 2 h to obtain refined lead - containing alkali slag; Transfer 40 g of refined lead - containing alkali slag to a converter, use natural gas - oxygen as fuel, add 80 g of modified porous anthracite, 60 g of iron filings, and 12 g of copper powder into the converter, melt at 1200 °C for 8 h, discharge the crude lead from the converter and slag. The crude lead from the converter enters a vacuum furnace after impurity removal in the impurity - removal process, and under the conditions of a vacuum degree of 30 Pa, a power of 310 kW, and a gas flow rate of 14 kg / min, perform vacuum separation to obtain a high - antimony lead based on refined lead - containing alkali slag.
[0033] Comparative Example 1: On the basis of Example S3, replace the porous anthracite in step S2 with the same mass of anthracite in step S1, and keep the other steps unchanged to prepare high - antimony lead.
[0034] Comparative Example 2: On the basis of Example S3, replace the modified porous anthracite in step S3 with the porous anthracite in step S2, and keep the other steps unchanged to prepare high - antimony lead.
[0035] Comparative Example 3: On the basis of Example S3, replace the zeolite - based modified asphalt powder in step S3 with the asphalt powder in step S3, and keep the other steps unchanged to prepare high - antimony lead.
[0036] In the examples and comparative examples: The alkali slag is purchased from Anhui Tianshuo Copper Powder Materials Co., Ltd.
[0037] The asphalt powder is purchased from Hebei Hankai Energy Technology Development Co., Ltd.
[0038] Perform performance tests on the high - antimony lead prepared in Examples 1 - 3 and Comparative Examples 1 - 3. The recycled refined lead produced is detected according to the standard of GB / T469 - 2005 to detect the recovery rate of antimony and the lead content in the slag, as shown in Table 1: Table 1 Performance Test Results of High-Antimony Lead
[0039] As can be seen from Table 1, for the high-antimony lead prepared in Examples 1-3, the lead content in the slag is lower than that in the comparative example, and the antimony recovery rate is significantly higher than that in the comparative example, indicating that the high-antimony lead prepared by the present invention has high antimony recovery rate, high efficiency, small slag volume, low lead content in the slag, small lead loss and high economic benefits.
[0040] In Comparative Example 1, the porous anthracite was replaced with anthracite. By intercalating urea between the anthracite layers, the interlayer spacing of the anthracite was increased. After carbonization, a porous structure was formed on the surface of the anthracite. The intercalated anthracite, due to the increase in interlayer spacing and the change in surface properties, can enhance the reduction ability.
[0041] In Comparative Example 2, the modified porous anthracite was replaced with porous anthracite. Nano-calcium oxide is an effective desulfurizer. After inserting nano-calcium oxide into the anthracite, it can react with sulfur dioxide generated during the production of high-antimony lead to form calcium sulfate, thereby fixing the sulfur element. The intercalation of nano-calcium oxide may also enhance the tolerance of anthracite. Nano-calcium oxide can protect the structure of anthracite from being damaged, thereby improving its stability and durability.
[0042] In Comparative Example 3, the zeolite-based modified asphalt powder was replaced with asphalt. Zeolite has high porosity and high specific surface area, which enables zeolite particles to form more contact points and bonding surfaces in the asphalt. These contact points and bonding surfaces increase the interaction force between the asphalt and the anthracite, thereby improving the bonding strength; zeolite particles can fill the microscopic pores and cracks in the asphalt, reduce the void ratio, and improve the compactness of the asphalt. This filling effect makes the contact between the asphalt and the aggregate closer, thereby improving the bonding strength. The spherical anthracite has a regular shape, which can reduce the resistance during the combustion process and make the combustion smoother, further improving the combustion efficiency.
[0043] The high-antimony lead prepared by the present invention has high purity, and a method for effectively recovering copper powder, antimony and lead from antimony-containing lead alkaline slag. This method has high drug utilization rate and avoids the problem of insufficient utilization rate of sodium hydroxide.
[0044] It should be noted that in this article, relational terms such as first and second are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variant thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements not only includes those elements, but also includes other elements not expressly listed, or also includes elements inherent to such process, method, article or device.
[0045] Although embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of the present invention, and the scope of the present invention is defined by the appended claims and their equivalents.
Claims
1. A high antimony lead production process based on lead refining alkali slag, characterized in that: Prepared by the following steps: Step 1: Add the modified porous anthracite and zeolite-based modified asphalt powder into a reaction kettle, stir at 135-140°C for 8-12 minutes, knead and process into a spherical shape, transfer to a muffle furnace, keep warm at 800-900°C for 4-6 hours under nitrogen protection, and cool naturally to obtain spherical modified porous anthracite with a particle size of 1-2 cm; Step 2: crushing the lead alkali slag, passing it through a 100-120 mesh sieve, and slurrying it with sodium hydroxide with a concentration of 80-85g / L, adding the slurry-adjusted material into a leaching tank, leaching it at 80-85°C for 2-3h, performing liquid-solid separation, and vacuum drying to obtain lead refined alkali slag; transferring the lead refined alkali slag to a converter, using natural gas-oxygen as fuel, adding modified porous anthracite, iron filings and copper powder into the converter, smelting at 1100-1200°C for 6-8h, releasing the converter crude lead and slag, and the converter crude lead is removed by a de-impurity process and then enters a vacuum furnace, performing vacuum separation under the conditions of a vacuum degree of 20-30pa, a power of 290-310kW, and a gas flow rate of 12-14kg / min, collecting high-antimony lead, and completing a high-antimony lead production process based on lead refined alkali slag.
2. The high antimony lead production process based on lead refining alkali slag according to claim 1, characterized in that: The usage ratio of the modified porous anthracite and the zeolite-based modified asphalt powder is 30-40g:4-5g.
3. The high antimony lead production process based on lead refining alkali slag according to claim 1, characterized in that: The usage ratio of the lead alkali slag and sodium hydroxide is 400-500g:3-4L.
4. The high antimony lead production process based on lead refining alkali slag according to claim 1, characterized in that: The usage ratio of the lead refining alkali slag, modified porous anthracite, iron filings and copper powder is 30-40g: 70-80g: 50-60g: 10-12g.
5. The high antimony lead production process based on lead refining alkali slag according to claim 1, characterized in that: The zeolite-based modified asphalt powder in step 1 is prepared by the following steps: Add asphalt powder with a particle size of 3-5 mm and sodium dodecyl sulfate into the reactor, keep warm at 135-140℃ for 20-30 min, then add zeolite powder, stir at 400-500r / min for 30-40 min, continue stirring and keeping warm for 15-20 min, shear at a rate of 3000-4000r / min for 1-2h, grind, cool naturally, and pass through an 80-100 mesh sieve to obtain zeolite-based modified asphalt powder.
6. The high antimony lead production process based on lead refining alkali slag according to claim 5, characterized in that: The mass ratio of the asphalt powder, sodium lauryl sulfate and zeolite is 20-23:1-2:4-5.
7. The high antimony lead production process based on lead refining alkali slag according to claim 1, characterized in that: The modified porous anthracite described in step 1 is prepared by the following steps: Add nano calcium oxide with a particle size of 50-100 nm and deionized water into a reactor, stir at 20-25° C. and 400-500 r / min for 30-40 min, ultrasonically disperse for 30-40 min, add porous anthracite, vacuum impregnate for 2-3 h at a temperature of 50-65° C. and a stirring rate of 400-500 r / min, cool naturally, stand for 24-26 h, filter, wash the filter cake with deionized water and anhydrous ethanol for 2-3 times respectively, and vacuum dry to obtain modified porous anthracite.
8. The process for producing high antimony lead based on lead refining alkali slag according to claim 7, characterized in that: The dosage ratio of the nano calcium oxide, deionized water and porous anthracite is 20-30 g: 300-400 mL: 20-23 g.
9. The high antimony lead production process based on lead refining alkali slag according to claim 7, characterized in that: The porous anthracite is prepared by the following steps: Add urea and deionized water into a reactor, stir at 20-25°C and 400-500r / min for 30-40min, crush the anthracite to 1-2mm, dry at 105-120°C for 2-3h, mix with sodium dodecyl sulfate and add into the reactor, vacuum impregnate at 50-65°C and 400-500r / min for 2-3h, filter, wash the filter cake with deionized water and anhydrous ethanol for 2-3 times respectively, vacuum dry, grind, pass through a 100-120 mesh sieve, transfer to a muffle furnace, keep warm at 800-900°C for 4-6h under nitrogen protection, cool naturally, and obtain porous anthracite.
10. The high antimony lead production process based on lead refining alkali slag according to claim 9, characterized in that: The usage ratio of urea, deionized water, sodium dodecyl sulfate and anthracite is 20-30 mL: 300-400 mL: 1-2 g: 30-40 g.
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