CN109988921A - The method of antimony is separated in a kind of hydrochloric acid-chloride solution - Google Patents
The method of antimony is separated in a kind of hydrochloric acid-chloride solution Download PDFInfo
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- CN109988921A CN109988921A CN201910309056.8A CN201910309056A CN109988921A CN 109988921 A CN109988921 A CN 109988921A CN 201910309056 A CN201910309056 A CN 201910309056A CN 109988921 A CN109988921 A CN 109988921A
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- antimony
- hydrochloric acid
- quinquevalence
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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
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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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/02—Obtaining antimony
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- 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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Abstract
The invention discloses a kind of methods that antimony is separated in hydrochloric acid-chloride solution, include: that oxidant is added into hydrochloric acid-chloride solution, controls reaction condition, the trivalent antimony in solution is made to be oxidized to quinquevalence antimony, and make quinquevalence antimony Precipitation pentavalent sb oxide, to obtain quinquevalence antimony oxide precipitation slurry；The quinquevalence antimony oxide precipitation slurry is aged, so that quinquevalence antimony oxide crystallization therein is grown up, is then separated by solid-liquid separation, to obtain quinquevalence antimony oxide solid and except solution after antimony, that is, realizes the separation of antimony.The present invention can not only efficient selective separation antimony, antimony recovery it is high, and process flow is simple, easy to operate.
Description
Technical field
The present invention relates to separate antimony in non-ferrous metal technical field of wet metallurgy more particularly to a kind of hydrochloric acid-chloride solution
Method.
Background technique
Currently, the smelting process of antimony can be divided into antimony pyrometallurgical smelting and antimony hydrometallurgy two major classes, based on antimony pyrometallurgical smelting.Pyrogenic process refining
Antimony is mainly blast furnace volatile smelting-reducing smelting process, i.e., first produces antimony oxide, restores again melting production needle antimony,
But this antimony pyrometallurgical smelting process metal rate of recovery is low, energy consumption is high, seriously polluted, especially low concentration SO2Flue gas and a large amount of arsenic alkali
Slag is all the main the difficult problem of environmental protection that antimony pyrometallurgical smelting faces.
Antimony hydrometallurgy is broadly divided into two methods of alkaline leaching antimony regulus and acidic leaching antimony regulus.Alkaline leaching antimony regulus is mainly
Vulcanized sodium leaching-thioantimonious acid sodium solution electrodeposition method, technique Na2S hyperplasia is serious, sodium sulphate, sodium thiosulfate, sulfurous
Sour sodium and schlippe's salt accumulation are serious, and liquid waste processing amount is big and more many and diverse, and for handling when containing Au-Sn deposit, golden leaching rate
Height easily causes the spread loss of gold.Acidic leaching antimony regulus is mainly studied in hydrochloric acid system, is equipped with such as chlorine, ferric trichloride, five
The different oxidant such as antimony chloride, ozone, or deoxidation leaching stibnite makes antimony enter solution by the way of electroxidation, obtains
To the leachate of chloride containing antimony, final antimony product is then made using the methods of Hydrolyze method or electrodeposition method；Hydrolyze method can be direct
Stibium trioxide is made, but a large amount of acid waste waters can be generated, reagent consumption is big, and electrodeposition method produces metallic antimony, ionic membrane valence used
Lattice are expensive, leach liquid acidity height, and foreign ion accumulating rate is fast in electrolyte, and it is big that electrolytic deposition process controls difficulty.
For the separation of antimony in hydrochloric acid system, patent CN108796219A discloses a kind of " extraction-in antimony iron mixed solution
Vulcanize the method for phase inversion separation antimony iron ", patent CN108728643A discloses a kind of " extraction-water decomposition in antimony iron mixed solution
The method for separating antimony and iron ", the common trait of this two patents are to turn antimony, iron ion in acid solution valence for low price, so
Low price antimony ion, iron ion extractibility qualitative difference are utilized afterwards, and the property selected extracts antimony into organic phase；The difference of this two patents exists
In to antimony organic phase is loaded, it is to directly obtain antimony trisulfide by vulcanizing phase inversion in first patent, is to pass through in second patent
Method for hydrolysis obtains antimony oxychloride；But reducing agent iron powder used in the method in this two patents introduces impurity, if for antimony
Extract technology so removes the method that iron burden is bigger, and furthermore the de- antimony of load organic phases uses generation solid antimonial, small
Solid grain is entrained in organic, it will influences extractant performance.Patent CN107557579B discloses a kind of " acid complicated containing antimony
The method of extraction and separation antimony iron in solution ", but the always time rate of antimony is lower, it is special the problem of separation in strip liquor there are still antimony, iron
Not in the presence of various metals impurity and various metals valence state, extraction selectivity is bad.
Summary of the invention
In order to solve to separate process flow complexity present in antimony, the recycling of antimony poor selectivity, antimony from acid solution at present
The low technical problem of rate, the present invention provides a kind of methods that antimony is separated in hydrochloric acid-chloride solution, can not only efficient selective
It is high to separate antimony, antimony recovery, and process flow is simple, easy to operate.
The purpose of the present invention is what is be achieved through the following technical solutions:
The method of antimony is separated in a kind of hydrochloric acid-chloride solution, comprising the following steps:
Oxidant is added into hydrochloric acid-chloride solution for step 1, controls reaction condition, is oxidized to the trivalent antimony in solution
Quinquevalence antimony, and make quinquevalence antimony Precipitation pentavalent sb oxide, to obtain quinquevalence antimony oxide precipitation slurry；
Step 2 is aged the quinquevalence antimony oxide precipitation slurry, keeps quinquevalence antimony oxide crystallization therein long
Greatly, it is then separated by solid-liquid separation, to obtain quinquevalence antimony oxide solid and except solution after antimony, that is, realizes the separation of antimony.
Preferably, contain antimony element in the hydrochloric acid-chloride solution, and wherein concentration of hydrochloric acid is 10~70g/L, chlorine
Salinity is 50~300g/L.
Preferably, the villaumite is at least one of calcium chloride, sodium chloride, magnesium chloride, potassium chloride；The oxidation
Agent is at least one of chlorine, hydrogen peroxide, ozone.
Preferably, in step 1, it is 30~60 DEG C that the control reaction condition, which includes: control reaction temperature, mixing speed
For 100~300rpm, the reaction time is 0.5~2 hour, and reaction end solution potential is greater than 700mV (vs.SHE), to make molten
Trivalent antimony in liquid is oxidized to quinquevalence antimony, and makes quinquevalence antimony Precipitation pentavalent sb oxide.
Preferably, in step 2, the quinquevalence antimony oxide precipitation slurry is aged, reaction temperature is 30~90
DEG C, mixing speed is 50~200rpm, and the reaction time is not less than 3 hours.
As seen from the above technical solution provided by the invention, antimony is separated in hydrochloric acid-chloride solution provided by the invention
Method concentration when being stabilized in hydrochloric acid-chloride solution for the antimony ion of different valence state difference, pass through oxidation
Promote trivalent antimony to be changed into the quinquevalence antimony for being easy to crystalline deposit, and quinquevalence antimony crystallization be precipitated by condition control, is aged and grows up,
The higher pentavalent sb oxide of purity is isolated from hydrochloric acid-chloride solution to realize, and can be in hydrochloric acid-chloride system
Efficiently separating for antimony and impurity element is realized during antimony electrolysis etc., and not only antimony is selectively good, but also antimony recovery is high, technique stream
Journey is simple, easy to operate.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Attached drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for this
For the those of ordinary skill in field, without creative efforts, it can also be obtained according to these attached drawings other
Attached drawing.
Fig. 1 is provided the flow diagram that the method for antimony is separated in hydrochloric acid-chloride solution by the embodiment of the present invention.
Fig. 2 is the pictorial diagram of obtained pentavalent sb oxide in the embodiment of the present invention 2.
Fig. 3 is the XRD diagram of obtained pentavalent sb oxide in the embodiment of the present invention 2.
Specific embodiment
With reference to the attached drawing in the embodiment of the present invention, technical solution in the embodiment of the present invention carries out clear, complete
Ground description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on this
The embodiment of invention, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, belongs to protection scope of the present invention.
The method that antimony is separated in hydrochloric acid-chloride solution provided by the present invention is described in detail below.The present invention is real
It applies the content being not described in detail in example and belongs to the prior art well known to professional and technical personnel in the field.
As shown in Figure 1, a kind of method for separating antimony in hydrochloric acid-chloride solution, it may include following steps:
Step 1, oxidation precipitation: oxidant is added into hydrochloric acid-chloride solution, and controls reaction condition, makes in solution
Trivalent antimony is oxidized to quinquevalence antimony, and makes quinquevalence antimony Precipitation pentavalent sb oxide, to obtain quinquevalence antimony oxide precipitation
Slurry.
Step 2, ageing are grown up: being aged to the quinquevalence antimony oxide precipitation slurry, aoxidized quinquevalence antimony therein
Object crystal growth, is then separated by solid-liquid separation, to obtain quinquevalence antimony oxide solid and except solution after antimony, that is, is realized from salt
Antimony is separated in acid-chloride solution.Present invention may also apply to the separation of the antimony iron of antimony iron mixed solution.Except the recyclable benefit of solution after antimony
With.
Specifically, it may include following embodiments that each step in the method for antimony is separated in the hydrochloric acid-chloride solution:
(1) in step 1, contain antimony element in the hydrochloric acid-chloride solution, such as: the hydrochloric acid-chloride solution
In may include the leachate of the raw material containing antimony, the leachate of antimony-containing mineral, the electrolyte in antimony electrorefining processes, antimony electro-deposition
Electrolyte etc. in the process.Concentration of hydrochloric acid is 10~70g/L in the hydrochloric acid-chloride solution, and villaumite concentration is 50~300g/
L.The villaumite is at least one of calcium chloride, sodium chloride, magnesium chloride, potassium chloride.
(2) in step 1, the oxidant is chlorine, hydrogen peroxide, ozone etc..
(3) in step 1, oxidant is added into hydrochloric acid-chloride solution, and controlling reaction temperature is 30~60 DEG C, is stirred
Mixing speed is 100~300rpm, and the reaction time is 0.5~2 hour, and reaction end solution potential is greater than 700mV (vs.SHE, phase
To standard hydrogen electrode), so that the trivalent antimony in solution be made to be oxidized to quinquevalence antimony, and aoxidize quinquevalence antimony Precipitation quinquevalence antimony
Object.
(4) in step 2, the quinquevalence antimony oxide precipitation slurry is aged, reaction temperature is 30~90 DEG C, is stirred
Mixing speed is 50~200rpm, and the reaction time is not less than 3 hours, so that quinquevalence antimony oxide crystallization be made to grow up.
Compared with prior art, the present invention has at least the following advantages:
(1) difference of concentration when the present invention is stabilized in hydrochloric acid-chloride solution for the antimony ion of different valence state, leads to
Peroxidation promotes trivalent antimony to be changed into the quinquevalence antimony for being easy to crystalline deposit, and quinquevalence antimony crystallization is precipitated, is aged and grows up, from
And it can realize efficiently separating for antimony and iron.
(2) present invention by oxidation precipitation and ageing grow up this two step can the higher sb oxide of output purity, relatively
Heavy antimony technique is hydrolyzed in existing, hydrochloric acid reagent consumption is few, antimony recovery is high, and does not generate a large amount of waste water.
(3) present invention process is simple, process is short, can directly obtain sb oxide product, antimony good separating effect, and has
The advantages that equipment investment is few, operating cost is low, reagent consumption is small.
(4) the present invention provides a kind of from hydrochloric acid-chloride solution separates the general character method of antimony, makes all kinds of antimony ores and contains
Antimony material can efficiently separate out antimony in hydrochloric acid-villaumite, can also be realized during hydrochloric acid-chloride system antimony electrolysis etc. antimony with
Impurity element efficiently separates.
To sum up, the embodiment of the present invention can not only efficient selective separation antimony, antimony recovery it is high, and process flow
Simply, easy to operate.
In order to more clearly from show technical solution provided by the present invention and generated technical effect, below with tool
Body embodiment is provided for the embodiments of the invention the method for separating antimony in hydrochloric acid-chloride solution and is described in detail.
Embodiment 1
Stibnite solution is leached to hydrochloric acid-ammonium chloride system to handle, wherein concentration of hydrochloric acid be 30g/L, calcium chloride it is dense
Degree is 200g/L, concentration of iron 10g/L, antimony concentration are 30g/L.A kind of method that antimony is separated in hydrochloric acid-chloride solution, specifically may be used
With the following steps are included:
Step 1a, oxidation precipitation: chlorine is added in Xiang Shangshu solution and carries out oxidation precipitation, 30 DEG C of reaction temperature, stirring is fast
Degree is 300rpm, and the reaction time is 0.5 hour, and control reaction end solution potential is greater than 800mV (vs.SHE), is made in solution
Trivalent antimony is oxidized to quinquevalence antimony, and makes quinquevalence antimony Precipitation pentavalent sb oxide, to obtain quinquevalence antimony oxide precipitation slurry
Material.
Step 2a, ageing is grown up: being aged to the obtained quinquevalence antimony oxide precipitation slurry of step 1a, reaction temperature
30 DEG C, mixing speed 100rpm, the reaction time 4 hours, quinquevalence antimony oxide crystallization therein is made to grow up, after being then aged
Slurry is filtered, to obtain quinquevalence antimony oxide solid and except solution after antimony.
Specifically, quinquevalence antimony oxide solid obtained by the embodiment of the present invention 1 is containing Sb after removing the crystallization water
69.02%, it is 28.23% containing O, containing Fe is 0.45%, is 0.16% containing Cl, the rate of deposition of antimony reaches 95.25%.
Embodiment 2
Stibnite solution is leached to hydrochloric acid-Calcium Chloride System to handle, wherein concentration of hydrochloric acid be 40g/L, calcium chloride it is dense
Degree is 250g/L, concentration of iron 20g/L, antimony concentration are 60g/L.A kind of method that antimony is separated in hydrochloric acid-chloride solution, specifically may be used
With the following steps are included:
Step 1b, oxidation precipitation: chlorine is added in Xiang Shangshu solution and carries out oxidation precipitation, 40 DEG C of reaction temperature, stirring is fast
Degree is 300rpm, and the reaction time is 1.5 hours, and control reaction end solution potential is greater than 900mV (vs.SHE), is made in solution
Trivalent antimony is oxidized to quinquevalence antimony, and makes quinquevalence antimony Precipitation pentavalent sb oxide, to obtain quinquevalence antimony oxide precipitation slurry
Material.
Step 2b, ageing is grown up: being aged to the obtained quinquevalence antimony oxide precipitation slurry of step 1b, reaction temperature
30 DEG C, mixing speed 100rpm, the reaction time 2 hours, quinquevalence antimony oxide crystallization therein is made to grow up, after being then aged
Slurry is filtered, to obtain quinquevalence antimony oxide solid and except solution after antimony.
Specifically, quinquevalence antimony oxide solid obtained by the embodiment of the present invention 2 is containing Sb after removing the crystallization water
68.83%, it is 26.47% containing O, containing Ca is 0.55%, is 2.10% containing Fe, is 0.23% containing Cl, the rate of deposition of antimony reaches
97.71%.The photo in kind of quinquevalence antimony oxide solid obtained by the embodiment of the present invention 2 is as shown in Figure 2.The embodiment of the present invention
The XRD diagram of quinquevalence antimony oxide solid obtained by 2 is as shown in Figure 3.
Embodiment 3
Hydrochloric acid-sodium chloride antimony electrorefining system electrolyte is handled, wherein concentration of hydrochloric acid is 30g/L, sodium chloride
Concentration is 150g/L, antimony concentration is 40g/L.The method of antimony is separated in a kind of hydrochloric acid-chloride solution, it may include following steps:
Step 1c, oxidation precipitation: chlorine is added in Xiang Shangshu solution and carries out oxidation precipitation, 50 DEG C of reaction temperature, stirring is fast
Degree is 300rpm, and the reaction time is 1 hour, and control reaction end solution potential is greater than 800mV (vs.SHE), makes three in solution
Valence antimony is oxidized to quinquevalence antimony, and makes quinquevalence antimony Precipitation pentavalent sb oxide, to obtain quinquevalence antimony oxide precipitation slurry.
Step 2c, ageing is grown up: being aged to the obtained quinquevalence antimony oxide precipitation slurry of step 1c, reaction temperature
40 DEG C, mixing speed 100rpm, the reaction time 3 hours, quinquevalence antimony oxide crystallization therein is made to grow up, after being then aged
Slurry is filtered, to obtain quinquevalence antimony oxide solid and except solution after antimony.
Specifically, quinquevalence antimony oxide solid obtained by the embodiment of the present invention 3 is containing Sb after removing the crystallization water
69.64%, it is 28.35% containing O, containing Na is 0.25%, is 0.25% containing Cl, the rate of deposition of antimony reaches 96.25%.
To sum up, the embodiment of the present invention can not only efficient selective separation antimony, antimony recovery it is high, and process flow
Simply, easy to operate.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Within the technical scope of the present disclosure, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Subject to enclosing.
Claims (5)
1. separating the method for antimony in a kind of hydrochloric acid-chloride solution, which comprises the following steps:
Oxidant is added into hydrochloric acid-chloride solution for step 1, controls reaction condition, the trivalent antimony in solution is made to be oxidized to pentavalent
Antimony, and make quinquevalence antimony Precipitation pentavalent sb oxide, to obtain quinquevalence antimony oxide precipitation slurry；
Step 2 is aged the quinquevalence antimony oxide precipitation slurry, so that quinquevalence antimony oxide crystallization therein is grown up, so
After be separated by solid-liquid separation, to obtain quinquevalence antimony oxide solid and except solution after antimony, that is, realize the separation of antimony.
2. separating the method for antimony in hydrochloric acid-chloride solution according to claim 1, which is characterized in that the hydrochloric acid-chlorine
Contain antimony element in salting liquid, and wherein concentration of hydrochloric acid is 10~70g/L, villaumite concentration is 50~300g/L.
3. separating the method for antimony in hydrochloric acid-chloride solution according to claim 1 or 2, which is characterized in that the villaumite
For at least one of calcium chloride, sodium chloride, magnesium chloride, potassium chloride；The oxidant is chlorine, in hydrogen peroxide, ozone
At least one.
4. separating the method for antimony in hydrochloric acid-chloride solution according to claim 1 or 2, which is characterized in that in step 1,
The control reaction condition includes: that control reaction temperature is 30~60 DEG C, and mixing speed is 100~300rpm, and the reaction time is
0.5~2 hour, reaction end solution potential was greater than 700mV (vs.SHE), so that the trivalent antimony in solution be made to be oxidized to pentavalent
Antimony, and make quinquevalence antimony Precipitation pentavalent sb oxide.
5. separating the method for antimony in hydrochloric acid-chloride solution according to claim 1 or 2, which is characterized in that in step 2,
The quinquevalence antimony oxide precipitation slurry is aged, reaction temperature is 30~90 DEG C, and mixing speed is 50~200rpm, instead
It is not less than 3 hours between seasonable.
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| CN201910309056.8A CN109988921B (en) | 2019-04-17 | 2019-04-17 | Method for separating antimony from hydrochloric acid-chlorine salt solution |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111074303A (en) * | 2020-01-19 | 2020-04-28 | 北京科技大学 | Method for separating antimony and gold by crude antimony non-anode-residue electrolysis |
| CN113089026A (en) * | 2021-03-17 | 2021-07-09 | 磨名言 | Method for electrolyzing and recovering antimony from antimony sulfide ore |
| CN114700339A (en) * | 2022-03-18 | 2022-07-05 | 大连理工大学 | Stabilization treatment method for iron-antimony waste residues |
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| JPS63282126A (en) * | 1987-05-11 | 1988-11-18 | Mitsubishi Metal Corp | Production of antimony oxide powder |
| CN101509079A (en) * | 2009-03-24 | 2009-08-19 | 中南大学 | Method for comprehensively processing stibium smelt arsenic alkaline residue and producing colloid antimony peroxide |
| CN105779789A (en) * | 2016-03-11 | 2016-07-20 | 中南大学 | Wet method for separating bismuth from antimony |
| CN105858724A (en) * | 2016-05-16 | 2016-08-17 | 中南大学 | Method of using solution atomization method to prepare superfine Sb oxide |
| CN109534396A (en) * | 2018-12-26 | 2019-03-29 | 浙江工业大学 | A kind of transition state sb oxide and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63282126A (en) * | 1987-05-11 | 1988-11-18 | Mitsubishi Metal Corp | Production of antimony oxide powder |
| CN101509079A (en) * | 2009-03-24 | 2009-08-19 | 中南大学 | Method for comprehensively processing stibium smelt arsenic alkaline residue and producing colloid antimony peroxide |
| CN105779789A (en) * | 2016-03-11 | 2016-07-20 | 中南大学 | Wet method for separating bismuth from antimony |
| CN105858724A (en) * | 2016-05-16 | 2016-08-17 | 中南大学 | Method of using solution atomization method to prepare superfine Sb oxide |
| CN109534396A (en) * | 2018-12-26 | 2019-03-29 | 浙江工业大学 | A kind of transition state sb oxide and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111074303A (en) * | 2020-01-19 | 2020-04-28 | 北京科技大学 | Method for separating antimony and gold by crude antimony non-anode-residue electrolysis |
| CN111074303B (en) * | 2020-01-19 | 2021-03-05 | 北京科技大学 | Method for separating antimony and gold by crude antimony non-anode-residue electrolysis |
| CN113089026A (en) * | 2021-03-17 | 2021-07-09 | 磨名言 | Method for electrolyzing and recovering antimony from antimony sulfide ore |
| CN114700339A (en) * | 2022-03-18 | 2022-07-05 | 大连理工大学 | Stabilization treatment method for iron-antimony waste residues |
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| CN109988921B (en) | 2021-09-14 |
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