CN102912155A - Recovery processing process of stanniferous electrofacing sludge - Google Patents
Recovery processing process of stanniferous electrofacing sludge Download PDFInfo
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- CN102912155A CN102912155A CN201210350379XA CN201210350379A CN102912155A CN 102912155 A CN102912155 A CN 102912155A CN 201210350379X A CN201210350379X A CN 201210350379XA CN 201210350379 A CN201210350379 A CN 201210350379A CN 102912155 A CN102912155 A CN 102912155A
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Abstract
The invention relates to a recovery processing process of stanniferous electrofacing sludge. The recovery processing process mainly comprises a leaching process and a replacement process. The leaching process comprises the following steps of: adding hydrochloric acid in the stanniferous electrofacing sludge, leaching contained tin elements to a solution, conducting solid-liquid separation and respectively obtaining a stanniferous solution and leaching slag; the replacement process comprises the following steps of: adding metallic aluminum materials in the stanniferous solution, and replacing to obtain sponge tin. The metal tin obtained by replacement is the sponge tin which obtains crude tin ingots through block pressing and ingot casting respectively, and the crude tin ingots are further purified through refining. Comprehensive recovery rate of the tin in the stanniferous electrofacing sludge can achieve 96%, aluminum entering the solution can be recovered through replacement in a followed treatment process, and waste water after aluminum recovery enters a pickling tank for circulation. An overall process can use waste acid, waste slag, waste water and waste aluminum to serve as raw materials, water steam of heat recovery boilers in a factory can be used for heating, and high-quality industrial raw materials can be produced. The waste slag is solidified according to national standards, and the waste slag can be used for filling after reaching the standard. The recovery processing process turns waste into wealth, saves energy and reduces discharge.
Description
Technical field
The present invention relates to a kind of recovery processing technique of stanniferous electroplating sludge.
Background technology
Tin belongs to little metal, and National Development and Reform Committee is conferring at present and classifying tin as China strategic reserves metal.China's tin reserves account for 28.85% of world's total reserves, and Yunnan Province of China Geju City is the tin ore enrichment region of present global known maximum, and wherein the tin resource reserves are more than 200 ten thousand tons.Yet because long-term, large-scale exploitation, the resource reserve that Gejiu Mine is verified seriously consumes.The mining area has 14 fairly large mines to close because resource exhaustion goes bankrupt, and has 4 to belong to Mine of Resources Crisis in 5 large-scale mines producing.Meanwhile, external original product tin big country Britain and Thailand, tin resource is also all exhausted.
Metallic tin purposes in industrial production is very extensive, and consumption is large, but some industry utilization ratio is not high.For example, some medium and small zinc-plated enterprise, the utilization ratio of tin is 40% only, causes a large amount of tin resource wastes.This just allows the comprehensive recovery of stanniferous electroplating sludge seem more urgent and important.Yet the prior art ubiquity rate of recovery is not high, can not comprehensively reclaim in the mud other metallic elements and reclaim in the problems such as resource consumption is larger.
In starting material, occurred so in short, far above the rate of recovery of other alkaline leaching and pickling process.That is to say that alkaline leaching and pickling process are routine techniquess, just our improvement by technique the rate of recovery, please the applicant is general introduce lower existing alkaline leaching and pickling process, and the dated device rate of recovery the chances are what?
The main flow process of alkaline leaching is: with leaching with sodium hydroxide-solid-liquid separation-evaporative crystallization output sodium stannate. this method leaching yield is low, leach total yield with secondary and also can only reach about 70%, and the sodium hydroxide price is high, and the sodium hydroxide consumption is large, and production cost is high.
Other has Introduction of Literatures with sulfuric acid leaching; because tin in the tin electroplating sludge is to exist with stannic hydroxide and two kinds of forms of simple substance tin; during sulfuric acid leaching; stannic hydroxide leaches easily; and the speed of dilute sulphuric acid dissolving simple substance tin is very slow; so when leaching the tin electroplating sludge with dilute sulphuric acid, the rate of recovery also is very low, can only reach 70% ~ 80%.
The present invention is with the finite concentration Leaching in Hydrochloric Acid, it is the characteristic that all can be dissolved in hydrochloric acid according to stannic hydroxide in the material and simple substance tin, one time leaching yield just can reach more than 95%, because leached mud only has 5%, leached mud is returned leaching, so total leaching yield is more than 99%. again with aluminium bits displacement tin, its rate of displacement is again more than 97%. with the spongy tin process washing that displaces, briquetting, ingot casting, obtain the tin slab more than 98%, total yield reaches more than 96%.
Summary of the invention
The object of the invention is to provide a kind of recovery processing technique of stanniferous electroplating sludge.
Purpose of the present invention is achieved through the following technical solutions: its key step comprises leaching process and replacement process, in the leaching process, hydrochloric acid is joined in the stanniferous electroplating sludge, tin element is wherein leached in the solution, through solid-liquid separation, obtain respectively containing solution of tin and leached mud; In the replacement process, the metallic aluminum material adding is contained in the solution of tin, displacement obtains spongy tin.
The metallic tin of getting in return is spongy tin, and spongy tin obtains thick tin slab through washing, briquetting, ingot casting respectively; Thick tin slab is further purified by refining.
Compared to prior art, the invention has the advantages that: adopt the technical program, the comprehensive recovery of tin can reach 96% in the stanniferous electroplating sludge, far above the rate of recovery of other alkaline leaching and pickling process; Its last handling process also reclaims the aluminium that displacement enters solution, takes full advantage of resource; Waste water behind the recovery aluminium can enter the pickling tank circulation; Whole process can be raw material with spent acid, waste residue, waste water, aluminium-foil scrap, and high-quality industrial raw material is produced in the exhaust steam heating of the waste heat boiler of available factory; The a small amount of waste gas that produces in the acidleach process can absorb through the liquid caustic soda spray column, and waste water circulation uses; Waste residue solidifies by GB, landfill up to standard.Having accomplished turns waste into wealth, energy-saving and emission-reduction.
Description of drawings
Fig. 1 reclaims the tin slab process flow sheet in the stanniferous mud.
Fig. 2 is the coordinate diagram of extraction temperature-leaching yield.
Fig. 3 is the coordinate diagram of concentration of hydrochloric acid-leaching yield.
Fig. 4 is displacement temperature-rate of displacement.
Embodiment
Below in conjunction with embodiment content of the present invention is elaborated:
As shown in Figure 1: its key step comprises leaching process and replacement process, it is characterized in that: in the leaching process, hydrochloric acid is joined in the stanniferous electroplating sludge, tin element is wherein leached in the solution, through solid-liquid separation, obtain respectively containing solution of tin and leached mud; In the replacement process, the metallic aluminum material adding is contained in the solution of tin, displacement obtains spongy tin.
Spongy tin obtains thick tin slab through washing, briquetting, ingot casting respectively; Thick tin slab is further purified by refining.
Adopt the hydrochloric acid of various typical concentrations all can implement among the present invention.For the increase operational security that simplifies the operation, reduce simultaneously exhaust gas emission, the preferably salt acid concentration is 1.5 ~ 3.5mol/L, the solid-liquid mass volume ratio that contains electroplating sludge and hydrochloric acid is 1kg:5 ~ 12L.
In leaching process, can carry out under the normal temperature, to improve temperature of reaction and help to improve speed of reaction, the prolongation reaction times helps to improve the leaching yield of tin.Preferred temperature of reaction is 60 ~ 99 ℃, and the reaction times is more than the 60min.
In order can to improve in the stanniferous electroplating sludge, the recovery of tin, leached mud generally mixes new stanniferous electroplating sludge and again leaches.Can guarantee like this leaching yield of tin more than 96% in the stanniferous electroplating sludge.
Described metallic aluminum material all can be realized for the various aluminiums take metallic aluminium as main component.Be to improve rate of displacement, the metallic aluminum material add-on can be slightly excessive, and preferred add-on is 1.1 ~ 1.5 times of tin amount of substance in the stanniferous electroplating sludge.For improving speed of reaction, metallic aluminum material is preferably powdery or laminar.
In replacement process, can carry out under the normal temperature, to improve temperature of reaction and help to improve speed of reaction, the prolongation reaction times helps to improve the rate of displacement of tin.Preferred temperature of reaction is 50 ~ 70 ℃, and the reaction times is more than the 60min.
For economizing on resources, protection of the environment as improvement, also can add last handling process in the recovery processing technique of the present invention: after displacement obtained tin, it was 10 ~ 12 that surplus solution is regulated PH, and solid-liquid separation obtains containing aluminum solutions and solid sediment; With the described aluminum solutions that contains, regulating PH is 3 ~ 6, obtains aluminum hydroxide precipitation, and aluminum hydroxide precipitation obtains aluminum oxide through calcination, landfill after solid sediment is cured and processes.
Regulate in the process of PH to 10 ~ 12, use highly basic commonly used to implement, below be a kind of preferred alkalization method: regulate first PH to 6 ~ 7 with lime, use again highly basic such as sodium hydroxide or potassium hydroxide to regulate PH to 10 ~ 12.
Regulating PH is that 3 ~ 6 acid commonly used of using can be implemented, such as sulfuric acid or hydrochloric acid.
The waste water that produces in the last handling process enters the leaching process circulation; The a small amount of waste gas that produces in leaching process absorbs through the liquid caustic soda spray column.
The principles of chemistry of the recovery processing technique of stanniferous electroplating sludge of the present invention are as follows: in leaching process, with the major metal Elements Leachings such as Sn, Fe, Ca, Cr, Mg in the stanniferous electroplating sludge to solution; In replacement process, use metallic aluminium, mainly the Sn in the solution is cemented out, obtain metallic tin; In the alkaline purification of last handling process, surplus solution is regulated PH to 10 ~ 12, make other metallic element except aluminium with the form of oxyhydroxide precipitation, obtain solid slag, aluminium element is then stayed in the solution with the aluminic acid ionic species; Be 3 ~ 6 through overregulating PH then, aluminium is precipitated with the aluminium hydroxide form.
In order further to prove advantage of the present invention, the applicant tests with regard to several committed steps.
One, leaching process
Test two: the selection of extraction temperature
Select 2.9mol/L concentration hydrochloric acid, under solid-to-liquid ratio 1kg:6L condition, under each temperature, react one hour leaching yield and test result such as table one, shown in Figure 2.
As shown in Table 1, leaching process at room temperature can carry out, and improves temperature of reaction and helps to improve speed of reaction, thereby improve the leaching yield in the same time.Extraction temperature is in 60 ~ 99 ℃, and leaching effect is better, surpasses 99 ℃ and produces more steam.
Test two: the selection of concentration of hydrochloric acid
Under 95 ℃, solid-to-liquid ratio 1kg:6L condition, adopt different concns hydrochloric acid, react and tested in one hour, result such as table two, shown in Figure 3.
As shown in Table 2, leaching process adopts each typical concentrations hydrochloric acid all can implement, and increases concentration of hydrochloric acid and helps to improve speed of reaction.For the increase operational security that simplifies the operation, reduce simultaneously waste gas, 1.5 ~ 3.5mol/L concentration can be satisfied the demand.
Two, replacement process
Under differing temps, in the same time, replace test with 1.3 times aluminium of tin amount of substance.Test-results sees Table three, shown in Figure 4.
As shown in Table 3, replacement process at room temperature can carry out, suitably improve temperature of reaction and help to improve speed of reaction, thereby improve rate of displacement in the same time, yet when temperature of reaction is too high, tin have certain return molten.Under 50 ~ 70 ℃, replacement result is better.
Three, last handling process
After displacement obtains tin, with surplus solution, regulate first PH to 6 ~ 7 with lime, regulate PH to 10 ~ 12 with sodium hydroxide again, solid-liquid separation obtains containing aluminum solutions and solid sediment; With the described aluminum solutions that contains, regulating PH with sulfuric acid is 3 ~ 6, obtains aluminum hydroxide precipitation, and aluminum hydroxide precipitation obtains aluminum oxide through calcination.The waste water that produces enters the leaching process circulation; The a small amount of waste gas that produces in leaching process absorbs through the liquid caustic soda spray column.
The present invention will be described below in conjunction with specific operation process
In 1 leaching process, 1.5mol/L hydrochloric acid is joined in the stanniferous electroplating sludge, in temperature is 99 ℃ environment, react 67min.The solid-liquid mass volume ratio that wherein contains electroplating sludge and hydrochloric acid is 1kg:11L, and tin element is wherein leached in the solution, through solid-liquid separation, obtains respectively containing solution of tin and leached mud; In the replacement process, metallic aluminum material added contain in the solution of tin, in temperature is 70 ℃ environment, reaction 60min.Wherein in the stanniferous electroplating sludge 1.2 times of the tin amount of substance, displacement obtains spongy tin.Spongy tin obtains thick tin slab through washing, briquetting, ingot casting respectively; Thick tin slab is further purified by refining.The rate of recovery of the tin that obtains here is 96.3%
Also can add last handling process in 2 recovery processing techniques: after displacement obtained tin, it was 11.2 that surplus solution is regulated PH, and control method is for to regulate first PH to 6.7 with lime, again with highly basic such as sodium hydroxide or potassium hydroxide adjusting PH to 11.2.Solid-liquid separation obtains containing aluminum solutions and solid sediment; With the described aluminum solutions that contains, regulating PH is 3.8, and regulating PH is 3.8 use hydrochloric acid.Obtain aluminum hydroxide precipitation, aluminum hydroxide precipitation obtains aluminum oxide through calcination, landfill after solid sediment is cured and processes.The waste water that produces in the last handling process enters the leaching process circulation; The a small amount of waste gas that produces in leaching process absorbs through the liquid caustic soda spray column.
In 1 leaching process, 3.5mol/L hydrochloric acid is joined in the stanniferous electroplating sludge, in temperature is 70 ℃ environment, react 60min.The solid-liquid mass volume ratio that wherein contains electroplating sludge and hydrochloric acid is 1kg:5L, and tin element is wherein leached in the solution, through solid-liquid separation, obtains respectively containing solution of tin and leached mud; In the replacement process, metallic aluminum material added contain in the solution of tin, in temperature is 60 ℃ environment, reaction 60min.Wherein in the stanniferous electroplating sludge 1.5 times of the tin amount of substance, displacement obtains spongy tin.Spongy tin obtains thick tin slab through washing, briquetting, ingot casting respectively; Thick tin slab is further purified by refining.The rate of recovery of the tin that obtains here is 96.8%
Also can add last handling process in 2 recovery processing techniques: after displacement obtained tin, it was 10.1 that surplus solution is regulated PH, and control method is for to regulate first PH to 7 with lime, again with highly basic such as sodium hydroxide or potassium hydroxide adjusting PH to 10.1.Solid-liquid separation obtains containing aluminum solutions and solid sediment; With the described aluminum solutions that contains, regulating PH is 6, and regulating PH is 6 use hydrochloric acid.Obtain aluminum hydroxide precipitation, aluminum hydroxide precipitation obtains aluminum oxide through calcination, landfill after solid sediment is cured and processes.The waste water that produces in the last handling process enters the leaching process circulation; The a small amount of waste gas that produces in leaching process absorbs through the liquid caustic soda spray column.
In 1 leaching process, 3.0mol/L hydrochloric acid is joined in the stanniferous electroplating sludge, in temperature is 60 ~ 99 ℃ environment, react 60min.The solid-liquid mass volume ratio that wherein contains electroplating sludge and hydrochloric acid is 1kg:12L, and tin element is wherein leached in the solution, through solid-liquid separation, obtains respectively containing solution of tin and leached mud; In the replacement process, metallic aluminum material added contain in the solution of tin, in temperature is 50 ℃ environment, reaction 68min.Wherein in the stanniferous electroplating sludge 1.1 times of the tin amount of substance, displacement obtains spongy tin.Spongy tin obtains thick tin slab through washing, briquetting, ingot casting respectively; Thick tin slab is further purified by refining.The rate of recovery of the tin that obtains here is 96.1%
Also can add last handling process in 2 recovery processing techniques: after displacement obtained tin, it was 12 that surplus solution is regulated PH, and control method is for to regulate first PH to 6 with lime, again with highly basic such as sodium hydroxide or potassium hydroxide adjusting PH to 12.Solid-liquid separation obtains containing aluminum solutions and solid sediment; With the described aluminum solutions that contains, regulating PH is 3, and regulating PH is 3 use sulfuric acid.Obtain aluminum hydroxide precipitation, aluminum hydroxide precipitation obtains aluminum oxide through calcination, landfill after solid sediment is cured and processes.The waste water that produces in the last handling process enters the leaching process circulation; The a small amount of waste gas that produces in leaching process absorbs through the liquid caustic soda spray column.
Claims (10)
1. the recovery processing technique of a stanniferous electroplating sludge, its step comprises leaching process and replacement process, it is characterized in that: in the leaching process, hydrochloric acid is joined in the stanniferous electroplating sludge, tin element is wherein leached in the solution, through solid-liquid separation, obtain respectively containing solution of tin and leached mud; In the replacement process, the metallic aluminum material adding is contained in the solution of tin, displacement obtains spongy tin.
2. the recovery processing technique of stanniferous electroplating sludge according to claim 1 is characterized in that: spongy tin obtains thick tin slab through washing, briquetting, ingot casting respectively; Thick tin slab is further purified by refining.
3. the recovery processing technique of stanniferous electroplating sludge according to claim 1, it is characterized in that: in the leaching process, temperature of reaction is 60 ~ 99 ℃, reaction times is more than the 60min, the concentration of hydrochloric acid is 1.5 ~ 3.5mol/L, and the solid-liquid mass volume ratio that contains electroplating sludge and hydrochloric acid is 1:5 ~ 12kg/L.
4. the recovery processing technique of stanniferous electroplating sludge according to claim 1 is characterized in that: leached mud mixes new stanniferous electroplating sludge and again leaches.
5. the recovery processing technique of stanniferous electroplating sludge according to claim 1 is characterized in that: described metallic aluminum material is the various aluminiums take metallic aluminium as main component, and add-on is 1.1 ~ 1.5 times of tin amount of substance in the stanniferous electroplating sludge.
6. the recovery processing technique of stanniferous electroplating sludge according to claim 5, it is characterized in that: described metallic aluminum material is powdery or laminar.
7. the recovery processing technique of stanniferous electroplating sludge according to claim 1, it is characterized in that: its replacement process, temperature of reaction are 50 ~ 70 ℃, the reaction times is more than the 60min.
8. the recovery processing technique of stanniferous electroplating sludge according to claim 1, it is characterized in that: it also comprises last handling process: after displacement obtained tin, it was 10 ~ 12 that surplus solution is regulated PH, and solid-liquid separation obtains containing aluminum solutions and solid sediment; Contain aluminum solutions to regulate PH be 3 ~ 6 described, obtain aluminum hydroxide precipitation, aluminum hydroxide precipitation obtains aluminum oxide through calcination, landfill after solid sediment is cured and processes.
9. the recovery processing technique of stanniferous electroplating sludge according to claim 8 is characterized in that: regulate in the process of PH to 10 ~ 12, regulate first PH to 6 ~ 7 with lime, regulate PH to 10 ~ 12 with sodium hydroxide or potassium hydroxide again; Regulating PH is that 3 ~ 6 acid of using are sulfuric acid or hydrochloric acid.
10. the recovery processing technique of stanniferous electroplating sludge according to claim 8 is characterized in that: the waste water that produces in the last handling process enters the leaching process circulation; The a small amount of waste gas that produces in leaching process absorbs through the liquid caustic soda spray column.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106435188A (en) * | 2016-08-30 | 2017-02-22 | 江苏省冶金设计院有限公司 | Treatment method and system for hot metallized pellets |
| CN108330297A (en) * | 2018-03-26 | 2018-07-27 | 赣州市赤鼎再生资源有限公司 | A kind of method that abandoned mine material recycles |
| CN109896721A (en) * | 2019-04-03 | 2019-06-18 | 宝武集团环境资源科技有限公司 | A kind of processing method of stanniferous sludge |
| CN110224115A (en) * | 2018-03-02 | 2019-09-10 | 华南理工大学 | A kind of lithium ion battery negative material and the preparation method and application thereof |
| CN110408784A (en) * | 2019-08-09 | 2019-11-05 | 江苏盟杰新能源科技有限公司 | A kind of tin reclaimer and its working method |
| CN113621821A (en) * | 2021-08-20 | 2021-11-09 | 金隆铜业有限公司 | Method for recovering metallic tin from lead-bismuth-removed Kaldo furnace slag |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106435188A (en) * | 2016-08-30 | 2017-02-22 | 江苏省冶金设计院有限公司 | Treatment method and system for hot metallized pellets |
| CN110224115A (en) * | 2018-03-02 | 2019-09-10 | 华南理工大学 | A kind of lithium ion battery negative material and the preparation method and application thereof |
| CN108330297A (en) * | 2018-03-26 | 2018-07-27 | 赣州市赤鼎再生资源有限公司 | A kind of method that abandoned mine material recycles |
| CN109896721A (en) * | 2019-04-03 | 2019-06-18 | 宝武集团环境资源科技有限公司 | A kind of processing method of stanniferous sludge |
| CN110408784A (en) * | 2019-08-09 | 2019-11-05 | 江苏盟杰新能源科技有限公司 | A kind of tin reclaimer and its working method |
| CN113621821A (en) * | 2021-08-20 | 2021-11-09 | 金隆铜业有限公司 | Method for recovering metallic tin from lead-bismuth-removed Kaldo furnace slag |
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Application publication date: 20130206 |