CN107475541A - Pre-separation lead, the method for indium in a kind of lead bottom of from - Google Patents

Pre-separation lead, the method for indium in a kind of lead bottom of from Download PDF

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Publication number
CN107475541A
CN107475541A CN201710846761.2A CN201710846761A CN107475541A CN 107475541 A CN107475541 A CN 107475541A CN 201710846761 A CN201710846761 A CN 201710846761A CN 107475541 A CN107475541 A CN 107475541A
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CN
China
Prior art keywords
lead
indium
separation
sodium
solution
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710846761.2A
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Chinese (zh)
Inventor
李城龙
张少广
陶家荣
徐宏凯
谭晓明
杨荣净
朱世波
陈凯
张泽林
赵永喜
杨勇斌
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
MAGUAN YUNTONG ZINC INDUSTRY Co Ltd
Original Assignee
MAGUAN YUNTONG ZINC INDUSTRY Co Ltd
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Priority to CN201710846761.2A priority Critical patent/CN107475541A/en
Publication of CN107475541A publication Critical patent/CN107475541A/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B58/00Obtaining gallium or indium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B13/00Obtaining lead
    • C22B13/02Obtaining lead by dry processes
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The present invention discloses pre-separation lead, the method for indium in a kind of lead bottom of from, wherein, including step:A, bottom lead is subjected to heating fusing and obtains fused solution, and the fused solution is maintained at predetermined temperature;B, sodium hydroxide, sodium nitrate and sodium chloride are added into the fused solution to be reacted, the bottom lead solution for containing scum silica frost in surface is obtained after reacting the scheduled time;C, the scum silica frost is pulled out from the bottom lead solution, realizes that the pre-separation of lead and indium solves the problems, such as that existing pyrometallurgy of zinc production midsole lead is difficult to be broken so as to cause valuable metal indium, lead cost recovery is high, the wasting of resources be present.

Description

Pre-separation lead, the method for indium in a kind of lead bottom of from
Technical field
The present invention relates to pre-separation lead, the method for indium in zinc abstraction field, more particularly to a kind of lead bottom of from.
Background technology
, can output bottom lead after steaming zinc and dragging for slag in existing pyrometallurgy of zinc production process.Bottom lead is more based on lead First alloy and metallic compound, due to containing valuable indium metal in the lead of bottom, be difficult to be broken again so that the recovery of indium metal and lead into This is higher, the rate of recovery is low.Bottom lead is caused to overstock in storehouse because the indium in bottom lead, lead do not have preferable recovery method for a long time Storehouse, cause certain wasting of resources.
Therefore, prior art has yet to be improved and developed.
The content of the invention
In view of above-mentioned the deficiencies in the prior art, it is an object of the invention to provide pre-separation lead in a kind of lead bottom of from, indium Method, it is intended to solve in existing pyrometallurgy of zinc production, caused bottom lead causes valuable metal indium, lead recovery because being difficult to be broken Cost is high, is deposited in warehouse for a long time and the problem of wasting of resources be present.
Technical scheme is as follows:
Pre-separation lead, the method for indium in a kind of lead bottom of from, wherein, including step:
A, bottom lead is subjected to heating fusing and obtains fused solution, and the fused solution is maintained at predetermined temperature;
B, sodium hydroxide, sodium nitrate and sodium chloride are added into the fused solution to be reacted, table is obtained after reacting the scheduled time Contain the bottom lead solution of scum silica frost in face;
C, the scum silica frost is pulled out from the bottom lead solution, realizes the pre-separation of lead and indium.
Pre-separation lead, the method for indium in the lead bottom of from, wherein, the predetermined temperature in the step A is 400-450 DEG C.
Pre-separation lead, the method for indium in the lead bottom of from, wherein, the addition of sodium hydroxide accounts for bottom lead in the step B The 20-25% of weight.
Pre-separation lead, the method for indium in the lead bottom of from, wherein, the addition of sodium nitrate accounts for bottom lead weight in the step B The 10-15% of amount.
Pre-separation lead, the method for indium in the lead bottom of from, wherein, the addition of sodium chloride accounts for bottom lead weight in the step B The 5-10% of amount.
Pre-separation lead, the method for indium in the lead bottom of from, wherein, the scheduled time described in the step B is 4-6 hours.
Pre-separation lead, the method for indium in the lead bottom of from, wherein, the heating fusion temperature in the step A is more than 500 ℃。
Pre-separation lead, the method for indium in the lead bottom of from, wherein, the reaction temperature in the step B is 450 DEG C.
Beneficial effect:The present invention carries out high temperature melting using by bottom lead, and sodium hydroxide, nitre are added into the bottom lead after fusing Sour sodium and sodium chloride are reacted is oxidized to indium acid sodium by indium metal(Na3InO3), now indium acid sodium be dissolved in sodium hydroxide and chlorine Change in the solution of sodium and form scum silica frost and separated with lead, obtained scum silica frost can reclaim wherein indium by wet-leaching, and lead can enter to advance One step refines or is prepared into lead bullion.Reduce the separation and recovery cost to indium, lead in bottom lead caused by pyrometallurgy of zinc, solve because Bottom lead overstock and caused by the wasting of resources the problem of.
Brief description of the drawings
Fig. 1 be the lead of the present invention bottom of from pre-separation lead, indium method preferred embodiment flow chart.
Embodiment
The invention provides a kind of method of pre-separation lead, indium in lead bottom of from, for make the purpose of the present invention, technical scheme and Effect is clearer, clear and definite, and the present invention is described in more detail below.It should be appreciated that specific embodiment described herein Only to explain the present invention, it is not intended to limit the present invention.
Referring to Fig. 1, Fig. 1 be pre-separation lead in a kind of lead bottom of from of the present invention, indium method flow chart, as illustrated, It includes step:
S1, bottom lead is carried out heating fusing obtain fused solution, and the fused solution is maintained at predetermined temperature;
S2, into the fused solution, addition sodium hydroxide, sodium nitrate and sodium chloride are reacted, and table is obtained after reacting the scheduled time Contain the bottom lead solution of scum silica frost in face;
S3, the scum silica frost pulled out from the bottom lead solution, realize the pre-separation of lead and indium.
Specifically, caused bottom lead during existing pyrometallurgy of zinc, its main component Pb 52.4%, Zn 2.36, In 31.6%, Ag 0.5%, Sn 5.3%, As 0.07%, Cu 5.5%.Because bottom lead is difficult to be broken, lead, indium are difficult to be separated, and lead Bottom lead is caused to be overstock in warehouse, so as to cause certain wasting of resources.
To solve the above problems, causing the indium in the lead of bottom to be separated with lead according to basic refining in the present invention, bottom lead is added Into melting furnace, the fusing point of major metal in the lead of bottom(156 DEG C of indium, 231 DEG C of tin, 327 DEG C of lead), when heating-up temperature is 500 DEG C, Bottom lead can be made, and all fusing obtains fused solution, by resulting fused solution temperature control at 400-450 DEG C, in the condition of stirring Down slowly by sodium hydroxide, sodium nitrate(Oxidant)It is added in the bottom lead of melting with sodium chloride, is obtained after reacting the scheduled time The bottom lead solution of scum silica frost is contained on surface, and the scum silica frost is pulled out from the bottom lead solution, realizes the pre-separation of lead and indium.
Preferably, the addition of sodium hydroxide accounts for the 20-25% of bottom lead weight in step S2 of the present invention.
Specifically, the dosage of sodium hydroxide decides the separation degree of indium and bottom lead, when the addition of sodium hydroxide is less than Bottom lead weight 20% when, the indium remained in lead can increase, and be unfavorable for indium and separated with lead.When the addition of sodium hydroxide Higher than bottom lead weight 25% when so that in fused solution substantial amounts of lead also be oxidized enters in scum silica frost, do not reach lead, indium separation Separating effect.
Preferably, the addition of sodium nitrate accounts for the 10-15% of bottom lead weight in step S2 of the present invention.
Specifically, sodium hydroxide is individually added into the lead fused solution of bottom, now lead hardly reacts with sodium hydroxide, But in the presence of having sodium nitrate, the nitric acid of molten condition is received with oxidisability, while sodium nitrate decomposes to give off oxygen and also had Oxidisability so that part lead is oxidized and entered in scum silica frost.When the addition of sodium nitrate is less than the 10% of bottom lead weight, anti- Sodium nitrate does not have oxidation effectiveness during answering, and is unfavorable for indium and is separated with lead.When the addition of sodium nitrate is higher than bottom lead weight Amount 15% when so that in fused solution substantial amounts of lead also be oxidized enters in scum silica frost, do not reach lead, indium separate separating effect.
Preferably, the addition of sodium chloride accounts for the 5-10% of bottom lead weight in step S2 of the present invention.
Specifically, indium is oxidized to indium acid sodium and is soluble in sodium hydroxide liquation and can also be dissolved in chlorine in fused solution Change in sodium, because the addition of sodium hydroxide during the course of the reaction is limited, can be made more by adding a certain amount of sodium chloride More indium acid sodium are entered in scum silica frost, so that the addition of the separation of lead, indium, and sodium chloride will not introduce new impurity.Work as chlorine When the addition of change sodium is less than the 5% of bottom lead weight, because addition is very few, solute effect is not had, is unfavorable for indium and is divided with lead From.When the addition of sodium chloride is higher than the 10% of bottom lead weight, the addition of sodium chloride excessively causes to waste.
Preferably, the scheduled time described in step S2 of the present invention is 4~6 hours.
Preferably, 450 DEG C of reaction temperature in step S2 of the present invention.
Specifically, sodium hydroxide and temperature control when sodium nitrate and sodium chloride are added after the fusing of bottom lead at 450 DEG C, when Temperature is too high, solubility increase of the indium in the lead of bottom, is unfavorable for the separation of indium and lead, meanwhile, sodium nitrate can be acute when temperature is too high It is strong to decompose generation nitric oxide and nitrogen dioxide toxic gas, it is unfavorable for operation.
The method of pre-separation lead in a kind of lead bottom of from of the present invention, indium is explained below by specific embodiment:
Embodiment 1
1 ton heavy of bottom lead is added in melting furnace, is warming up to 500 DEG C, making bottom lead, all fusing obtains fused solution, control melting The temperature of liquid is at 400 DEG C, while stirring slowly into fused solution, adds sodium hydroxide 200kg, sodium nitrate 100kg, sodium chloride 50kg, the scum silica frost on bottom lead solution upper strata is pulled out after reacting 4h, realizes the pre-separation of lead and indium.Now, remain in fused solution Indium account for the 1% of total indium amount.
Embodiment 2
1 ton heavy of bottom lead is added in melting furnace, is warming up to 510 DEG C, making bottom lead, all fusing obtains fused solution, control melting The temperature of liquid is at 430 DEG C, while stirring slowly into fused solution, adds sodium hydroxide 220kg, sodium nitrate 130kg, sodium chloride 80kg, the scum silica frost on bottom lead solution upper strata is pulled out after reacting 5h, realizes the pre-separation of lead and indium.Now, remain in fused solution Indium account for the 0.7% of total indium amount.
Embodiment 3
1 ton heavy of bottom lead is added in melting furnace, is warming up to 520 DEG C, making bottom lead, all fusing obtains fused solution, control melting The temperature of liquid is at 450 DEG C, while stirring slowly into fused solution, adds sodium hydroxide 250kg, sodium nitrate 150kg, sodium chloride 100kg, the scum silica frost on bottom lead solution upper strata is pulled out after reacting 6h, realizes the pre-separation of lead and indium.Now, remain in fused solution Indium account for the 0.5% of total indium amount.
In summary, the present invention carries out high temperature melting using by bottom lead, and sodium hydroxide, nitre are added into the bottom lead after fusing Sour sodium and sodium chloride are reacted is oxidized to indium acid sodium by indium metal(Na3InO3), now indium acid sodium be dissolved in sodium hydroxide and chlorine Change in the solution of sodium and form scum silica frost and separated with lead, obtained scum silica frost can reclaim wherein indium by wet-leaching, and lead can enter to advance One step refines or is prepared into lead bullion.Reduce the separation and recovery cost to indium, lead in bottom lead caused by pyrometallurgy of zinc, solve because Bottom lead overstock and caused by the wasting of resources the problem of.
It should be appreciated that the application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can To be improved or converted according to the above description, all these modifications and variations should all belong to the guarantor of appended claims of the present invention Protect scope.

Claims (8)

1. pre-separation lead, the method for indium in a kind of lead bottom of from, it is characterised in that including step:
A, bottom lead is subjected to heating fusing and obtains fused solution, and the fused solution is maintained at predetermined temperature;
B, sodium hydroxide, sodium nitrate and sodium chloride are added into the fused solution to be reacted, table is obtained after reacting the scheduled time Contain the bottom lead solution of scum silica frost in face;
C, the scum silica frost is pulled out from the bottom lead solution, realizes the pre-separation of lead and indium.
2. pre-separation lead, the method for indium in the lead according to claim 1 bottom of from, it is characterised in that pre- in the step A Constant temperature degree is 400-450 DEG C.
3. pre-separation lead, the method for indium in the lead according to claim 1 bottom of from, it is characterised in that hydrogen-oxygen in the step B The addition for changing sodium accounts for the 20-25% of bottom lead weight.
4. pre-separation lead, the method for indium in the lead according to claim 1 bottom of from, it is characterised in that nitric acid in the step B The addition of sodium accounts for the 10-15% of bottom lead weight.
5. pre-separation lead, the method for indium in the lead according to claim 1 bottom of from, it is characterised in that chlorination in the step B The addition of sodium accounts for the 5-10% of bottom lead weight.
6. pre-separation lead, the method for indium in the lead according to claim 1 bottom of from, it is characterised in that described in the step B The scheduled time is 4-6 hours.
7. pre-separation lead, the method for indium in the lead according to claim 1 bottom of from, it is characterised in that adding in the step A Heat fusing temperature is more than 500 DEG C.
8. according to claim 1 from the lead of bottom pre-separation lead, indium method, it is characterised in that the reaction in the step B Temperature is 450 DEG C.
CN201710846761.2A 2017-09-19 2017-09-19 Pre-separation lead, the method for indium in a kind of lead bottom of from Pending CN107475541A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110055419A (en) * 2019-04-06 2019-07-26 柳州呈奥科技有限公司 A kind of preparation method based on recovery indium in zinc metallurgy byproduct
CN114507782A (en) * 2022-02-14 2022-05-17 郴州云湘矿冶有限责任公司 Method and system for recycling indium from indium-containing soldering tin

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110055419A (en) * 2019-04-06 2019-07-26 柳州呈奥科技有限公司 A kind of preparation method based on recovery indium in zinc metallurgy byproduct
CN114507782A (en) * 2022-02-14 2022-05-17 郴州云湘矿冶有限责任公司 Method and system for recycling indium from indium-containing soldering tin
CN114507782B (en) * 2022-02-14 2024-03-22 郴州云湘矿冶有限责任公司 Method and system for recycling indium from indium-containing soldering tin

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Application publication date: 20171215