阅读说明：本技术 一种利用火法除铋精炼精铅的方法 (Method for removing bismuth and refining refined lead by pyrogenic process ) 是由 张璐盈 陈甦 花丽明 娄可柏 戢习武 刘飞 罗秋月 于 2020-10-12 设计创作，主要内容包括：本发明涉及一种利用火法除铋精炼精铅的方法,包括如下步骤：将精铅装入精炼锅中进行高温熔化捞出熔化渣；(2)将温度控制在580-610℃,中速搅拌加入钙铝合金,持续搅拌,使钙铝合金与铅液充分混合并产生浮渣上浮至铅液表面,慢速搅拌8-15分钟,凝固成粒状渣浮于铅液表面,捞出浮渣；(3)用水降温冷却至430-450℃,中速搅拌的同时加入镁粉,静止存放8-15分钟；(4)自然降温至320-360℃加入铅锑合金,搅拌,控制温度320-350℃,中速搅拌8-15分钟；静放10-20分钟,捞出表面壳状铅铋渣；(5)铅液升温至420-450℃加入氢氧化钠,溶液中的锡形成含锡的碱性浮渣,捞出锡渣,搅拌除锑至渣变成黄红色,再放入硝酸钠除镁,至铅液亮白色,捞出渣。本方法除铋效果显著,同时能量消耗低。(The invention relates to a method for removing bismuth by a pyrogenic process and refining refined lead, which comprises the following steps: putting the refined lead into a refining pot, melting at high temperature, and fishing out melted slag; (2) controlling the temperature at 580-610 ℃, adding the calcium-aluminum alloy by stirring at medium speed, continuously stirring to fully mix the calcium-aluminum alloy with the lead liquid and generate scum which floats to the surface of the lead liquid, stirring at low speed for 8-15 minutes to solidify into granular slag which floats to the surface of the lead liquid, and fishing out the scum; (3) cooling to 430-450 deg.C with water, adding magnesium powder while stirring at medium speed, standing and storing for 8-15 min; (4) naturally cooling to the temperature of 320-; standing for 10-20 minutes, and fishing out the surface shell-shaped lead-bismuth slag; (5) heating the lead liquid to 420 ℃ and 450 ℃, adding sodium hydroxide, forming tin-containing alkaline floating slag by tin in the solution, fishing out tin slag, stirring to remove antimony until the slag turns yellow-red, adding sodium nitrate to remove magnesium until the lead liquid is bright white, and fishing out the slag. The method has obvious bismuth removing effect and low energy consumption.)

1. A method for removing bismuth and refining refined lead by a pyrogenic process is characterized by comprising the following steps:

(1) putting the refined lead into a refining pot, melting at high temperature, and fishing out melted slag;

(2) controlling the temperature at 580-610 ℃, adding the calcium-aluminum alloy by stirring at medium speed, continuously stirring to fully mix the calcium-aluminum alloy with the lead liquid and generate scum which floats to the surface of the lead liquid, stirring at low speed for 8-15 minutes to solidify into granular slag which floats to the surface of the lead liquid, and fishing out the scum;

(3) cooling to 430-450 deg.C with water, adding magnesium powder while stirring at medium speed, standing and storing for 8-15 min;

(4) naturally cooling to the temperature of 320-; standing for 10-20 minutes, and fishing out the surface shell-shaped lead-bismuth slag;

(5) heating the lead liquid to 420-450 ℃, adding sodium hydroxide, forming tin-containing alkaline floating slag by tin in the solution, fishing out tin slag, stirring to remove antimony until the slag turns yellow-red, adding sodium nitrate to remove magnesium until the lead liquid is bright white, fishing out slag, and finishing bismuth refined lead ingot casting.

2. The method for removing bismuth by pyrogenic process according to claim 1, wherein: in the step (2), the frequency of medium-speed stirring is 18-30 Hz.

3. The method for removing bismuth by pyrogenic process according to claim 1, wherein: and (3) in the step (2), continuously stirring at medium speed in the process of cooling with water.

4. The method for removing bismuth by pyrogenic process according to claim 1, wherein: in the above steps, the stirring process is completed by using a stirrer.

5. The method for removing bismuth by pyrogenic process according to claim 1, wherein: in the above step, the temperature is reduced while stirring in step (4).

Technical Field

The invention relates to the technical field of fire refining refined lead, in particular to a method for refining refined lead by removing bismuth through a fire method.

Background

In the modern industrial field, such as the manufacturing field of lead storage batteries, the consumption of lead is very large, the bismuth impurity is often generated in the lead smelting process in the current metallurgical technological process, the content of bismuth in refined lead is too high, the method for removing bismuth from refined lead is not a lot in the prior art, and the invention is proposed to solve the problem.

Disclosure of Invention

The invention aims to provide a method for refining refined lead by removing bismuth by a pyrogenic process.

The technical problem to be solved by the invention is realized by adopting the following technical scheme:

a method for removing bismuth by a pyrogenic process to refine refined lead comprises the following steps:

(1) putting the refined lead into a refining pot, melting at high temperature, and fishing out melted slag;

(2) controlling the temperature at 580-610 ℃, adding the calcium-aluminum alloy by stirring at medium speed, continuously stirring to fully mix the calcium-aluminum alloy with the lead liquid and generate scum which floats to the surface of the lead liquid, stirring at low speed for 8-15 minutes to solidify into granular slag which floats to the surface of the lead liquid, and fishing out the scum;

(3) cooling to 430-450 deg.C with water, adding magnesium powder while stirring at medium speed, standing and storing for 8-15 min;

(4) naturally cooling to the temperature of 320-; standing for 10-20 minutes, and fishing out the surface shell-shaped lead-bismuth slag;

(5) heating the lead liquid to 420-450 ℃, adding sodium hydroxide, forming tin-containing alkaline floating slag by tin in the solution, fishing out tin slag, stirring to remove antimony until the slag turns yellow-red, adding sodium nitrate to remove magnesium until the lead liquid is bright white, fishing out slag, and finishing bismuth refined lead ingot casting.

In some embodiments, the frequency of moderate agitation in step (2) is 18-23 Hz.

Preferably, in the step (3), stirring at a medium speed is continuously carried out during the cooling process of water, and a large amount of slag is generated during the stirring process.

Preferably, the agitation is accomplished using a blender.

And (4) cooling while stirring.

Has the advantages that:

compared with the input and output by using the method, the method has the advantages that the yield of refined lead is high, the Bi content is reduced, the Bi content is obviously reduced, the bismuth removing effect is obvious, and the electric quantity consumption is low.

Detailed Description

In order to facilitate understanding of the technical means and the process flow of the present invention, the present invention is further described below with reference to specific embodiments.

Example 1:

preparing 3.5 tons of refined lead, 5kg of calcium-aluminum alloy, 12kg of magnesium powder, 50kg of lead-antimony alloy (with 10 percent of antimony), 18kg of sodium hydroxide and 9kg of sodium nitrate, and primarily sampling and analyzing the refined lead to obtain the following components: 0.02% of Sns; 0.00096% of Cu0; as0.00025%; ag0.00049 percent; sb0.00033%; bi0.025 percent; the balance being lead.

A method for refining refined lead by removing bismuth through a fire method comprises the following steps: (1) putting the refined lead into a refining pot, melting at high temperature, and fishing out melted slag; (2) controlling the temperature at 580 ℃, stirring at a rotating speed of 18Hz, adding the calcium-aluminum alloy, continuously stirring to fully mix the calcium-aluminum alloy and the lead liquid and generate scum which floats to the surface of the lead liquid, fishing out the scum, continuously stirring at a low speed for 8 minutes, solidifying into granular slag which floats to the surface of the lead liquid, and fishing out the scum; sampling and analyzing: ca0.095%; 0.013 percent of Sns; bi0.022%; (3) cooling to 450 ℃ with water, continuously stirring at a medium speed in the cooling process with water, adding magnesium powder while stirring at the medium speed, standing for 10 minutes, and sampling to analyze Mg0.324%; (4) naturally cooling to 360 ℃, adding lead-antimony alloy, stirring, controlling the temperature to 350 ℃, and stirring at medium speed for 8 minutes; sampling and analyzing: bi0.0027%; sb0.026%; standing for 20 minutes, fishing out the surface slag liquid, fishing out, and sampling and analyzing Bi0.0032%; (5) heating the lead liquid to 420 ℃, adding sodium hydroxide, absorbing tin in the solution to form sodium stannous, changing the sodium stannous into tin-containing alkaline floating slag, fishing out tin slag, stirring to remove antimony until the slag becomes yellowish red, adding sodium nitrate to remove magnesium until the lead liquid is bright white, fishing out slag, and finishing bismuth-removed refined lead ingot casting.

Example 2:

preparing 3.0 tons of refined lead, 4.5kg of calcium-aluminum alloy, 10kg of magnesium powder, 40kg of lead-antimony alloy (with 9 percent of antimony), 15kg of sodium hydroxide and 8kg of sodium nitrate, and primarily sampling and analyzing the refined lead to obtain the following components: 0.018% of Sns; 0.0009% of Cu0; as0.00026%; ag0.00041 percent; sb0.00035%; bi0.024%; the balance being lead.

A method for refining refined lead by removing bismuth through a fire method comprises the following steps: (1) putting the refined lead into a refining pot, melting at high temperature, and fishing out melted slag; (2) controlling the temperature at 580 ℃, adding the calcium-aluminum alloy under medium-speed stirring (23Hz), continuously stirring to fully mix the calcium-aluminum alloy with the lead liquid and generate scum which floats to the surface of the lead liquid, fishing out the scum, continuously stirring at low speed for 15 minutes, solidifying into granular slag which floats to the surface of the lead liquid, and fishing out the scum; sampling and analyzing: ca0.096%; 0.02% of Sns; bi0.021%; (3) cooling to 430 ℃ by using water, adding magnesium powder while stirring at medium speed, standing for 15 minutes, and sampling to analyze Mg0.328%; (4) naturally cooling to 320 ℃, adding lead-antimony alloy, stirring, controlling the temperature to 332 ℃, and stirring at medium speed for 15 minutes; sampling and analyzing: bi0.0027%; sb0.04%; standing for 10 minutes, fishing out the surface slag liquid, fishing out, sampling and analyzing Bi0.0032%; (5) heating the lead liquid to 450 ℃, adding sodium hydroxide, absorbing tin in the solution to form sodium stannous, changing the sodium stannous into tin-containing alkaline floating slag, fishing out tin slag, stirring to remove antimony until the slag becomes yellowish red, adding sodium nitrate to remove magnesium until the lead liquid is bright white, fishing out slag, and finishing bismuth-removed refined lead ingot casting.

Example 3:

preparing 3.5 tons of refined lead, 5kg of calcium-aluminum alloy, 12kg of magnesium powder, 50kg of lead-antimony alloy (with 10 percent of antimony), 18kg of sodium hydroxide and 9kg of sodium nitrate, and primarily sampling and analyzing the refined lead to obtain the following components: 0.02% of Sns; 0.00096% of Cu0; as0.00025%; ag0.00049 percent; sb0.00033%; bi0.025 percent; the balance being lead.

A method for refining refined lead by removing bismuth through a fire method comprises the following steps: (1) putting the refined lead into a refining pot, melting at high temperature, and fishing out melted slag; (2) controlling the temperature at 580 ℃, adding the calcium-aluminum alloy under medium-speed stirring (20Hz), continuously stirring to fully mix the calcium-aluminum alloy with the lead liquid and generate scum which floats to the surface of the lead liquid, fishing out the scum, continuously stirring at low speed for 10 minutes to solidify into granular slag which floats to the surface of the lead liquid, and fishing out the scum; sampling and analyzing: ca0.096%; 0.02% of Sns; bi0.021%; (3) cooling to 443 deg.C with water, adding magnesium powder while stirring at medium speed, standing for 10 min, and sampling to analyze Mg0.327%; (4) naturally cooling to 339 ℃, adding lead-antimony alloy, stirring, controlling the temperature to 332 ℃, and stirring at medium speed for about 10 minutes; sampling and analyzing: bi0.0028%; sb0.03%; taking out the surface slag liquid, and sampling and analyzing Bi0.0031%; and (5) heating the lead liquid to 440 ℃, adding sodium hydroxide, absorbing tin in the solution to form sodium stannous, changing the sodium stannous into tin-containing alkaline scum, fishing out the tin slag, stirring to remove antimony until the slag becomes yellowish red, adding sodium nitrate to remove magnesium until the lead liquid is bright white, fishing out the slag, and finishing bismuth refined lead ingot casting.

After the reaction is finished, weighing tests show that 3.5 tons of fine lead, 5kg of calcium-aluminum alloy, 12kg of magnesium powder, 50kg of lead-antimony alloy, 18kg of sodium hydroxide, 9kg of sodium nitrate and 3594 in total are added, 300 degrees of electric energy is consumed, fine lead 3040 is produced, 500 waste residues are produced, the yield is 0.86857, the yield is high, and meanwhile, the Bi content is obviously reduced through the sampling analysis and comparison of the front and back Bi contents.

The foregoing shows the general principles and features of the present invention and its advantages. While the foregoing embodiments and description have been made only for the purpose of illustrating the principles of the invention, and other details have not been set forth in detail, it will be apparent that various changes and modifications can be made therein without departing from the spirit and scope of the invention, which is defined by the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.