CN107099668A - A kind of alkaline antimony-containing solution deep removal copper, the method for lead - Google Patents

A kind of alkaline antimony-containing solution deep removal copper, the method for lead Download PDF

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CN107099668A
CN107099668A CN201710376107.XA CN201710376107A CN107099668A CN 107099668 A CN107099668 A CN 107099668A CN 201710376107 A CN201710376107 A CN 201710376107A CN 107099668 A CN107099668 A CN 107099668A
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lead
antimony
containing solution
copper
alkaline
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CN107099668B (en
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杨兴文
涂相林
祝志兵
邹志武
钟志燕
罗标
赵云峰
刘海华
罗钊荣
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Jiangxi Copper Corp
Jiangxi Copper Co Ltd
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Jiangxi Copper Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B30/00—Obtaining antimony, arsenic or bismuth
    • C22B30/02—Obtaining antimony
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Chemical Kinetics & Catalysis (AREA)
  • Environmental & Geological Engineering (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses a kind of method of alkaline antimony-containing solution deep removal copper, lead, comprise the following steps：1) composition silicate is added as additive and reacted in alkaline antimony-containing solution；2) separation of solid and liquid after reacting, liquid after obtaining copper, lead collection slag and handling, liquid is to remove the antimony-containing solution after copper, lead after the processing.The present invention uses CaSiO3·MgSiO3Compound, copper, the lead element in solution, and addition CO can be removed well under certain process conditions2Technique is passed through as selection process, follow-up CO2Gas removes the Mg deviate from compound2+、Ca2+, new impurity element will not be introduced, the antimony purity finally obtained is high.

Description

A kind of alkaline antimony-containing solution deep removal copper, the method for lead
Technical field
The invention belongs to non-ferrous metal metallurgy technical field, more particularly to a kind of alkaline antimony-containing solution deep removal copper, lead Method.
Background technology
Metallic antimony due to its property the characteristics of in addition to for electroplating, seldom be used alone, matched somebody with somebody more using other metals as matrix Into various alloys.19 beginnings of the century, antimony is used to manufacture shrapnel as the hardening agent of lead.With the lead containing antimony since 20th century Accumulator grid, stereotype and joint part are done, the consumption of antimony is increased, and with the development of Modern Traffic cause. The wear-resisting lead-antimony alloy of Babbitt of nineteen thirty-nine American invention, the bearing shell for making bearing, also known as bearing metal, in application process In continue to develop.Having the babbit of tinbase, lead base, zinc-base and aluminium antimony magnesium now is used for various different purposes.In addition, purity Antimony more than 99.9994%, for manufacture far infrared device, intermetallic compound semiconductor (such as BSb, AlSb, ZnSb, GaSb, InSb, CdSb etc.) it is alternatively arranged as dopant.
The smelting process of antimony includes：Antimony pyrometallurgical smelting, reduction melting and pyro-refining, electrorefining, precipitation melting, antimony oxide Ore smelting, the melting of Refractory Sb-Pb Concentrate stone and hydrometallurgy refinement method etc., in above-mentioned several method, easy can be applied to processing Low-grade complex antimong-containing material, and cost is low, high income method is that hydrometallurgy refines method.It is a kind of that hydrometallurgy, which refines method, Utilize the enrichment of hydrometallurgy means, the methods for extracting low-grade antimong-containing material antimony element such as acidleach, alkali leaching.
But during application alkali leaching method, in the leaching process of later stage antimony, leachate often has higher basicity, causes portion Divide copper, lead element to enter in leachate, and with entering in final antimony product, influence the quality of product.
The content of the invention
To solve the shortcoming and defect of prior art, the invention provides a kind of alkaline antimony-containing solution deep removal copper, lead Method, using the method can depth remove alkali soak method refine antimony-containing solution in copper, lead element.
To achieve the above object, the technical solution adopted by the present invention is：A kind of alkaline antimony-containing solution deep removal copper, lead Method, it is characterised in that comprise the following steps：
1) composition silicate is added as additive and reacted in leachate containing antimony；
2) separation of solid and liquid after reacting, liquid after obtaining copper, lead collection slag and handling, liquid is to remove after copper, lead after the processing Antimony-containing solution.
Further, the alkaline antimony-containing solution deep removal copper, the method for lead, its step is specially：
1) composition silicate is added as additive and reacted in alkaline antimony-containing solution, the addition quality of additive and Liquor capacity ratio is 5~50g/L, and reaction temperature is 30~95 DEG C, reaction time >=1 hour, and separation of solid and liquid after reaction is obtained Liquid after copper, lead collection slag and processing, liquid is to remove the antimony-containing solution after copper, lead after the processing；
2) it is passed through CO into liquid after processing2The flow of gas, wherein carbon dioxide ensures, in 1~5L/min, to be passed through CO2's Amount is 14~70g/L with liquor capacity ratio, and ventilation is filtered after finishing, and is obtained antimony-containing solution and is entered subsequent handling.
Preferably, OH in the alkaline antimony-containing solution-Concentration >=100g/L of ion.
Preferably, the addition quality of the additive and liquor capacity ratio are 30~40g/L, reaction temperature is 70~ 95℃。
Preferably, the composition silicate is added before leachate containing antimony, be first immersed in mass fraction be 5%~ More than 5min in 15% barium chloride solution, dries composition silicate after immersion at a temperature of 90~150 DEG C, then 400 1~2h is calcined at~550 DEG C, air cooling is taken out after calcining.
Further, the composition silicate is CaSiO3·MgSiO3Compound.
Further, the CaSiO3·MgSiO3The preparation process of compound is：
A. by SiO2Powder, CaO powder and MgO powder in mass ratio 2~3:2:1 proportioning is uniformly mixed, will after mixing Mixed-powder carries out ball milling, wherein batch mixing：The mass ratio of ball is 1~2：2, Ball-milling Time be 5~10h, rotating speed be 400~ 500r/min；
B. the batch mixing after ball milling is sieved, the mesh of the screen cloth >=1000；
C. the powder after sieving is calcined, the calcining heat is 1200~1400 DEG C, calcination time is 3~4h, Batch mixing is taken out after the completion of calcining and is air-cooled to room temperature；
D. the material after calcining is subjected to ball milling particle, wherein batch mixing：The mass ratio of ball is 1~2：2, Ball-milling Time be 10~ 20min, rotating speed is 400~500r/min, after ball milling both the CaSiO3·MgSiO3Compound.
The beneficial effects of the invention are as follows：
1. the copper, lead element in antimony-containing solution can enter final antimony product in subsequent processes with antimony element, make Copper, lead content are exceeded into follow-up antimony product, do not reach standard value.At higher basicities (alkaline leaching is utilized from antimong-containing material Leachate containing antimony obtained by middle leaching is respectively provided with high-alkali angle value), copper, lead element exist in forms such as copper acid group, plumbic acid roots, this hair Bright use CaSiO3·MgSiO3Compound, the copper that can be gone well in solution under certain process conditions, lead element are protected The quality and qualification rate of follow-up antimony product are demonstrate,proved.
2. the present invention uses CO2Gas remove the Mg that deviates from compound2+、Ca2+, new impurity element will not be introduced, It is follow-up to leach the antimony purity height obtained.
3. present invention process is simple, the requirement to equipment very place is low, it is easy to penetration and promotion.By optimizing CaSiO3· MgSiO3The preparation technology parameter of compound so that the compound copper removal of acquisition, lead best results.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing There is the accompanying drawing used required in technology description to be briefly described, it should be apparent that, drawings in the following description are only this Some embodiments of invention, for those of ordinary skill in the art, without having to pay creative labor, may be used also To obtain other accompanying drawings according to these accompanying drawings.
Fig. 1 is flow chart of the invention.
Embodiment
With reference to embodiment, the present invention will be further described, it should be understood that these embodiments are only used for illustration Purpose, be in no way intended to limit protection scope of the present invention.
As shown in figure 1, the invention discloses a kind of method of alkaline antimony-containing solution deep removal copper, lead, including following step Suddenly：
1) composition silicate is added as additive and reacted in leachate containing antimony；
2) separation of solid and liquid after reacting, liquid after obtaining copper, lead collection slag and handling, liquid is to remove after copper, lead after the processing Antimony-containing solution.
Embodiment 1
A kind of alkaline antimony-containing solution deep removal copper, the method for lead, its step is specially：
1) by CaSiO3·MgSiO3Composition silicate is added as additive to be reacted in alkaline antimony-containing solution, is added The addition quality of agent is 5g/L with liquor capacity ratio, and reaction temperature is 30 DEG C, 1 hour reaction time, and separation of solid and liquid after reaction is obtained Liquid after to copper, lead collection slag and processing, liquid is to remove the antimony-containing solution after copper, lead after the processing；
2) it is passed through CO into liquid after processing2Gas removes Mg present in solution2+、Ca2+, wherein carbon dioxide flow protect Card is passed through CO in 1~5L/min2Amount and liquor capacity ratio be 14g/L, ventilation is filtered after finishing, and is obtained antimony-containing solution and is entered Subsequent handling.
The content of the copper, lead, magnesium and the calcium constituent that have handled rear solution is determined using atomic absorption spectrophotometry, its As a result it is as shown in table 1.
Above-mentioned CaSiO3·MgSiO3The preparation process of composition silicate is：
A. by SiO2Powder, CaO powder and MgO powder in mass ratio 2:2:1 proportioning is uniformly mixed, will mixing after mixing Powder carries out ball milling, wherein batch mixing：The mass ratio of ball is 1：2, Ball-milling Time is 5h, and rotating speed is 400r/min；
B. the batch mixing after ball milling is sieved, the screen cloth is 1000 mesh；
C. the powder after sieving is calcined, the calcining heat is 1200 DEG C, and calcination time is 3h, after the completion of calcining Batch mixing is taken out and is air-cooled to room temperature；
D. the material after calcining is subjected to ball milling particle, wherein batch mixing：The mass ratio of ball is 1：2, Ball-milling Time is 10min, Rotating speed be after 450r/min, ball milling both the CaSiO3·MgSiO3Compound.
Embodiment 2
A kind of alkaline antimony-containing solution deep removal copper, the method for lead, its step is specially：
1) by CaSiO3·MgSiO3Composition silicate is added as additive to be reacted in alkaline antimony-containing solution, is added The addition quality of agent and liquor capacity ratio are 10g/L, and reaction temperature is 40 DEG C, the reaction time is 1 hour, solid-liquid point after reaction From, liquid after obtaining copper, lead collection slag and handling, liquid is to remove the antimony-containing solution after copper, lead after the processing；
2) it is passed through CO into liquid after processing2Gas removes Mg present in solution2+、Ca2+, wherein carbon dioxide flow protect Card is passed through CO in 1~5L/min2Amount and liquor capacity ratio be 30g/L, ventilation is filtered after finishing, and is obtained antimony-containing solution and is entered Subsequent handling.
The content of the copper, lead, magnesium and the calcium constituent that have handled rear solution is determined using atomic absorption spectrophotometry, its As a result it is as shown in table 1.
Above-mentioned CaSiO3·MgSiO3The preparation process of composition silicate is：
A. by SiO2Powder, CaO powder and MgO powder in mass ratio 2:2:1 proportioning is uniformly mixed, will mixing after mixing Powder carries out ball milling, wherein batch mixing：The mass ratio of ball is 1：2, Ball-milling Time is 6h, and rotating speed is 450r/min；
B. the batch mixing after ball milling is sieved, the mesh of screen cloth 1000；
C. the powder after sieving is calcined, the calcining heat is 1200 DEG C, and calcination time is 3h, after the completion of calcining Batch mixing is taken out and is air-cooled to room temperature；
D. the material after calcining is subjected to ball milling particle, wherein batch mixing：The mass ratio of ball is 1：2, Ball-milling Time is 10min, Rotating speed be after 450r/min, ball milling both the CaSiO3·MgSiO3Compound.
Embodiment 3
A kind of alkaline antimony-containing solution deep removal copper, the method for lead, its step is specially：
1) by CaSiO3·MgSiO3Composition silicate is added as additive to be reacted in alkaline antimony-containing solution, is added The addition quality of agent and liquor capacity ratio are 20g/L, and reaction temperature is 60 DEG C, the reaction time is 1 hour, solid-liquid point after reaction From, liquid after obtaining copper, lead collection slag and handling, liquid is to remove the antimony-containing solution after copper, lead after the processing；
2) it is passed through CO into liquid after processing2Gas removes Mg present in solution2+、Ca2+, wherein carbon dioxide flow protect Card is passed through CO in 1~5L/min2Amount and liquor capacity ratio be 30g/L, ventilation is filtered after finishing, and is obtained antimony-containing solution and is entered Subsequent handling.
The content of the copper, lead, magnesium and the calcium constituent that have handled rear solution is determined using atomic absorption spectrophotometry, its As a result it is as shown in table 1.
Above-mentioned CaSiO3·MgSiO3The preparation process of composition silicate is：
A. by SiO2Powder, CaO powder and MgO powder in mass ratio 2.5:2:1 proportioning is uniformly mixed, will be mixed after mixing Close powder and carry out ball milling, wherein batch mixing：The mass ratio of ball is 2：2, Ball-milling Time is 6h, and rotating speed is 450r/min；
B. the batch mixing after ball milling is sieved, the screen cloth is 1000 mesh；
C. the powder after sieving is calcined, the calcining heat is 1300 DEG C, and calcination time is 3h, after the completion of calcining Batch mixing is taken out and is air-cooled to room temperature；
D. the material after calcining is subjected to ball milling particle, wherein batch mixing：The mass ratio of ball is 2：2, Ball-milling Time is 15min, Rotating speed be after 450r/min, ball milling both the CaSiO3·MgSiO3Compound.
Embodiment 4
A kind of alkaline antimony-containing solution deep removal copper, the method for lead, its step is specially：
1) by CaSiO3·MgSiO3Composition silicate is added as additive to be reacted in alkaline antimony-containing solution, is added The addition quality of agent and liquor capacity ratio are 30g/L, and reaction temperature is 70 DEG C, the reaction time is 1 hour, solid-liquid point after reaction From, liquid after obtaining copper, lead collection slag and handling, liquid is to remove the antimony-containing solution after copper, lead after the processing；
2) it is passed through CO into liquid after processing2Gas removes Mg present in solution2+、Ca2+, wherein carbon dioxide flow protect Card is passed through CO in 1~5L/min2Amount and liquor capacity ratio be 60g/L, ventilation is filtered after finishing, and is obtained antimony-containing solution and is entered Subsequent handling.
The content of the copper, lead, magnesium and the calcium constituent that have handled rear solution is determined using atomic absorption spectrophotometry, its As a result it is as shown in table 1.
Above-mentioned CaSiO3·MgSiO3The preparation process of composition silicate is：
A. by SiO2Powder, CaO powder and MgO powder in mass ratio 3:2:1 proportioning is uniformly mixed, will mixing after mixing Powder carries out ball milling, wherein batch mixing：The mass ratio of ball is 2：2, Ball-milling Time is 6h, and rotating speed is 450r/min；
B. the batch mixing after ball milling is sieved, the screen cloth is 1000 mesh；
C. the powder after sieving is calcined, the calcining heat is 1300 DEG C, and calcination time is 3h, after the completion of calcining Batch mixing is taken out and is air-cooled to room temperature；
D. the material after calcining is subjected to ball milling particle, wherein batch mixing：The mass ratio of ball is 2：2, Ball-milling Time is 20min, Rotating speed be after 450r/min, ball milling both the CaSiO3·MgSiO3Compound.
Embodiment 5
A kind of alkaline antimony-containing solution deep removal copper, the method for lead, its step is specially：
1) by CaSiO3·MgSiO3Composition silicate is added as additive to be reacted in alkaline antimony-containing solution, is added The addition quality of agent and liquor capacity ratio are 40g/L, and reaction temperature is 80 DEG C, the reaction time is 1 hour, solid-liquid point after reaction From, liquid after obtaining copper, lead collection slag and handling, liquid is to remove the antimony-containing solution after copper, lead after the processing；
2) it is passed through CO into liquid after processing2Gas removes Mg present in solution2+、Ca2+, wherein carbon dioxide flow protect Card is passed through CO in 1~5L/min2Amount and liquor capacity ratio be 70g/L, ventilation is filtered after finishing, and is obtained antimony-containing solution and is entered Subsequent handling.
The content of the copper, lead, magnesium and the calcium constituent that have handled rear solution is determined using atomic absorption spectrophotometry, its As a result it is as shown in table 1.
Above-mentioned CaSiO3·MgSiO3The preparation process of composition silicate is：
A. by SiO2Powder, CaO powder and MgO powder in mass ratio 3:2:1 proportioning is uniformly mixed, will mixing after mixing Powder carries out ball milling, wherein batch mixing：The mass ratio of ball is 2：2, Ball-milling Time is 10h, and rotating speed is 450r/min；
B. the batch mixing after ball milling is sieved, the screen cloth is 1000 mesh；
C. the powder after sieving is calcined, the calcining heat is 1400 DEG C, and calcination time is 4h, after the completion of calcining Batch mixing is taken out and is air-cooled to room temperature；
D. the material after calcining is subjected to ball milling particle, wherein batch mixing：The mass ratio of ball is 2：2, Ball-milling Time is 20min, Rotating speed be after 450r/min, ball milling both the CaSiO3·MgSiO3Compound.
Embodiment 6
A kind of alkaline antimony-containing solution deep removal copper, the method for lead, its step is specially：
1) by CaSiO3·MgSiO3Composition silicate is added as additive to be reacted in alkaline antimony-containing solution, is added The addition quality of agent and liquor capacity ratio are 50g/L, and reaction temperature is 95 DEG C, the reaction time is 1 hour, solid-liquid point after reaction From, liquid after obtaining copper, lead collection slag and handling, liquid is to remove the antimony-containing solution after copper, lead after the processing；
2) it is passed through CO into liquid after processing2Gas removes Mg present in solution2+、Ca2+, wherein carbon dioxide flow protect Card is passed through CO in 1~5L/min2Amount and liquor capacity ratio be 60g/L, ventilation is filtered after finishing, and is obtained antimony-containing solution and is entered Subsequent handling.
The content of the copper, lead, magnesium and the calcium constituent that have handled rear solution is determined using atomic absorption spectrophotometry, its As a result it is as shown in table 1.
Above-mentioned CaSiO3·MgSiO3The preparation process of composition silicate is：
A. by SiO2Powder, CaO powder and MgO powder in mass ratio 3:2:1 proportioning is uniformly mixed, will mixing after mixing Powder carries out ball milling, wherein batch mixing：The mass ratio of ball is 2：2, Ball-milling Time is 6h, and rotating speed is 450r/min；
B. the batch mixing after ball milling is sieved, the screen cloth is 1000 mesh；
C. the powder after sieving is calcined, the calcining heat is 1300 DEG C, and calcination time is 3h, after the completion of calcining Batch mixing is taken out and is air-cooled to room temperature；
D. the material after calcining is subjected to ball milling particle, wherein batch mixing：The mass ratio of ball is 2：2, Ball-milling Time is 20min, Rotating speed be after 450r/min, ball milling both the CaSiO3·MgSiO3Compound.
Comparative example 1
A kind of alkaline antimony-containing solution deep removal copper, the method for lead, its operating procedure and the technological parameter such as institute of embodiment 4 State, it is differed only in：Step 1) in watery hydrochloric acid by the PH of antimony-containing solution regulation to acid (i.e. PH≤7), other techniques are joined Number is identical with embodiment 4 with method.
Copper, lead, magnesium and the calcium constituent for having handled rear solution are determined after having handled using atomic absorption spectrophotometry Content, its result is as shown in table 1.
Comparative example 2
A kind of alkaline antimony-containing solution deep removal copper, the method for lead, its operating procedure and the technological parameter such as institute of embodiment 4 State, it is differed only in：Step 1) in the PH of antimony-containing solution regulation arrived into alkalescent (PH is 12) with watery hydrochloric acid, other techniques are joined Number is identical with embodiment 4 with method.
Copper, lead, magnesium and the calcium constituent for having handled rear solution are determined after having handled using atomic absorption spectrophotometry Content, its result is as shown in table 1.
Comparative example 3
A kind of alkaline antimony-containing solution deep removal copper, the method for lead, its operating procedure and the technological parameter such as institute of embodiment 4 State, it is differed only in：The step 2) in, by CaSiO3·MgSiO3Composition silicate is added before alkaline antimony-containing solution, first 5min in the barium chloride solution that mass fraction is 10% is immersed in, is dried composition silicate at a temperature of 90 DEG C after immersion, so Air cooling is taken out after calcining 1h, calcining at 450 DEG C afterwards.
Copper, lead, magnesium and the calcium constituent for having handled rear solution are determined after having handled using atomic absorption spectrophotometry Content, its result is as shown in table 1.
Comparative example 4
A kind of alkaline antimony-containing solution deep removal copper, the method for lead, its operating procedure and the technological parameter such as institute of embodiment 4 State, it is differed only in：The step 2) in CaSiO3·MgSiO3With etc. quality CaSiO3Powder is replaced, other techniques Parameter is identical with embodiment 4 with method.
Copper, lead, magnesium and the calcium constituent for having handled rear solution are determined after having handled using atomic absorption spectrophotometry Content, its result is as shown in table 1.
Comparative example 5
A kind of alkaline antimony-containing solution deep removal copper, the method for lead, its operating procedure and the technological parameter such as institute of embodiment 4 State, it is differed only in：The step 2) in CaSiO3·MgSiO3With etc. quality MgSiO3Powder is replaced, other techniques Parameter is identical with embodiment 4 with method.
Copper, lead, magnesium and the calcium constituent for having handled rear solution are determined after having handled using atomic absorption spectrophotometry Content, its result is as shown in table 1.
Comparative example 6
A kind of alkaline antimony-containing solution deep removal copper, the method for lead, its operating procedure and the technological parameter such as institute of embodiment 4 State, it is differed only in：The step 2) in CaSiO3·MgSiO3Equally used according to the mole of Ca, Mg element CaSiO3And MgSiO3Powder is replaced, and other technological parameters are identical with embodiment 4 with method.
Copper, lead, magnesium and the calcium constituent for having handled rear solution are determined after having handled using atomic absorption spectrophotometry Content, its result is as shown in table 1.
Table 1
As can be seen from Table 1, using CaSiO3·MgSiO3Copper, lead meeting in the alkaline antimony-containing solution of composition silicate removing A certain amount of Ca and Mg ions are introduced, therefore the present invention uses and is passed through CO2Mode Ca, Mg are removed as preferred side Case.From table from the point of view of experimental result, with CO2Ca, Mg content are reduced in the increase of intake, solution, when intake reaches During more than 30g/L, effect is notable.Ca, Mg content after processing in solution can not influence subsequent technique with up to standard completely.
The content highest of copper, lead element in liquid containing antimony is up to 2g/L.Knowable to 1~embodiment of comparative example 6, this hair Cu, Pb content is significantly reduced in alkaline antimony-containing solution after the reason of daylight, copper, lead content can as little as below 50mg/L, can make Enter next step production line for acceptable material.CaSiO3·MgSiO3The addition quality and reaction temperature of complex silicate salt additives Removal effect influence on copper, lead is very big, when addition quality and the liquor capacity ratio of additive are 30~40g/L, reaction temperature For 70~95 DEG C when, effect preferably, the copper-lead in solution can be fully apparent from substantially.
Knowable to comparative example 4 and comparative example 1, comparative example 2, CaSiO of the present invention3·MgSiO3Composition silicate adds Plus agent only just has good effect under the environment of alkalescence, sour environment does not remove Cu, Pb technique effect substantially, and Technique effect is also undesirable under weakly alkaline environment, does not reach the requirement needed for industrial production.
Comparative example 4 and comparative example 3 are understood, complex silicate salt additives of the present invention are entered using barium chloride solution Row pre-treatment can further improve the activity that additive removes Cu, Pb, and this is probably because Ba forms copper on additive Lead binding site, easy and copper-lead forms stable complex salt, is further exacerbated by Cu, Pb precipitation abjection.
Comparative example 4 and comparative example 4~6 are understood, merely using CaSiO3Solid, MgSiO3Solid or CaSiO3、 MgSiO3Physical mixed do not have removing antimony solution in copper and lead technique effect, CaSiO3Solid, MgSiO3Solid simple substance There is no the active site position that Cu, Pb are combined, add after being reacted completely in solution and still keep CaSiO3Solid, MgSiO3Solid is original Structure, form and surface state.

Claims (7)

1. a kind of alkaline antimony-containing solution deep removal copper, the method for lead, it is characterised in that comprise the following steps：
1) composition silicate is added as additive and reacted in alkaline antimony-containing solution；
2) separation of solid and liquid after reacting, liquid after obtaining copper, lead collection slag and handling, liquid is to remove containing after copper, lead after the processing Antimony solution.
2. a kind of alkaline antimony-containing solution deep removal copper according to claim 1, the method for lead, it is characterised in that it is walked It is rapid to be specially：
1) composition silicate is added as additive and reacted in alkaline antimony-containing solution, the addition quality and solution of additive Volume ratio is 5~50g/L, and reaction temperature is 30~95 DEG C, reaction time >=1 hour, and separation of solid and liquid after reaction obtains copper, lead Collect liquid after slag and processing, liquid is to remove the antimony-containing solution after copper, lead after the processing；
2) it is passed through CO into liquid after processing2The flow of gas, wherein carbon dioxide ensures, in 1~5L/min, to be passed through CO2Amount with Liquor capacity ratio is 14~70g/L, and ventilation is filtered after finishing, and is obtained antimony-containing solution and is entered subsequent handling.
3. a kind of alkaline antimony-containing solution deep removal copper according to claim 2, the method for lead, it is characterised in that described OH in alkaline antimony-containing solution-Concentration >=100g/L of ion.
4. a kind of alkaline antimony-containing solution deep removal copper according to claim 2, the method for lead, it is characterised in that described The addition quality of additive is 30~40g/L with liquor capacity ratio, and reaction temperature is 70~95 DEG C.
5. a kind of alkaline antimony-containing solution deep removal copper according to claim 2, the method for lead, it is characterised in that described Composition silicate is added before alkaline antimony-containing solution, is first immersed in 5min in the barium chloride solution that mass fraction is 5%~15% More than, composition silicate is dried at a temperature of 90~150 DEG C after immersion, 1~2h, calcining are then calcined at 400~550 DEG C After take out air cooling.
6. a kind of alkaline antimony-containing solution deep removal copper according to any one of Claims 1 to 5, the method for lead, its feature It is, the composition silicate is CaSiO3·MgSiO3Compound.
7. a kind of alkaline antimony-containing solution deep removal copper according to claim 6, the method for lead, it is characterised in that described CaSiO3·MgSiO3The preparation process of compound is：
A. by SiO2Powder, CaO powder and MgO powder in mass ratio 2~3:2:1 proportioning is uniformly mixed, by mixed powder after mixing End carries out ball milling, wherein batch mixing：The mass ratio of ball is 1~2：2, Ball-milling Time is 5~10h, and rotating speed is 400~500r/min；
B. the batch mixing after ball milling is sieved, the mesh of the screen cloth >=1000；
C. the powder after sieving is calcined, the calcining heat is 1200~1400 DEG C, calcination time is 3~4h, calcining After the completion of by batch mixing take out be air-cooled to room temperature；
D. the material after calcining is subjected to ball milling particle, wherein batch mixing：The mass ratio of ball is 1~2：2, Ball-milling Time be 10~ 20min, rotating speed is 400~500r/min, after ball milling both the CaSiO3·MgSiO3Compound.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0102044A2 (en) * 1982-08-27 1984-03-07 Süd-Chemie Ag Agent containing thiolate and process for removing heavy metal ions from diluted aqueous solutions
CN1194237A (en) * 1997-03-24 1998-09-30 张至德 Wet process for preparing industrial pure antimony sulfide by removing load, arsenic, selenium, tin and mercury impurities in antimonic ore
CN105274565A (en) * 2014-07-18 2016-01-27 张超 Method for electrolyzing metals through wet method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0102044A2 (en) * 1982-08-27 1984-03-07 Süd-Chemie Ag Agent containing thiolate and process for removing heavy metal ions from diluted aqueous solutions
CN1194237A (en) * 1997-03-24 1998-09-30 张至德 Wet process for preparing industrial pure antimony sulfide by removing load, arsenic, selenium, tin and mercury impurities in antimonic ore
CN105274565A (en) * 2014-07-18 2016-01-27 张超 Method for electrolyzing metals through wet method

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