CN107574301B - From the method for Leaching of Antimony manganese simultaneously in stibnite and pyrolusite - Google Patents
From the method for Leaching of Antimony manganese simultaneously in stibnite and pyrolusite Download PDFInfo
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- CN107574301B CN107574301B CN201710971041.9A CN201710971041A CN107574301B CN 107574301 B CN107574301 B CN 107574301B CN 201710971041 A CN201710971041 A CN 201710971041A CN 107574301 B CN107574301 B CN 107574301B
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Abstract
The method of Leaching of Antimony manganese simultaneously that the invention discloses a kind of from stibnite and pyrolusite, it is leached simultaneously comprising steps of 1) be placed in stibnite in hydrochloric acid solution with pyrolusite, then ore pulp will be leached and carry out solid-liquor separation, obtain the leachate I and sulfur-bearing leached mud containing antimony manganese salt solution, 2) add antimony powder reduction into leachate I, obtain the leachate II based on antimony trichloride and manganese chloride, 3) leachate II is hydrolyzed, and can get antimony oxychloride hydrolysis residue and manganese chloride solution after solid-liquor separation.Present invention Leaching of Antimony manganese simultaneously from stibnite and pyrolusite using wet processing effectively prevents the problems such as production environment is poor, sulfur dioxide pollution is serious during pyrometallurgical smelting.This method is suitable for low-grade stibnite and pyrolusite, to improve the increasingly utilization rate of the antimony ore and manganese resource of dilution, reduction environmental pollution.
Description
Technical field
The invention belongs to field of metallurgy and chemical engineering, and in particular to a kind of method that stibnite leaches simultaneously with pyrolusite.
Background technique
With the high speed development of current world economy and science and technology, the application field of antimony is more and more extensive, can be used for producing
Various fire retardants, glass, rubber, semiconductor element etc..Currently, antimony fire retardant is the main application fields of antimony, account for about world's antimony
The 70% of sales volume.China is antimony resource big country, the world, and antimony product specie, yield occupy first place in the world.Stibnite is main antimony deposit,
It is one kind with Sb2S3Based on sulphide ore.The method that stibnite extracts antimony mainly has pyrogenic process and two kinds of wet process, thermal process master
It to be made of volatile smelting and reduction melting, the extraction efficiency of antimony is relatively high, but production environment is poor, low-concentration oxidizing sulphur pollution
It is serious etc..With going deep into for green production theory, the strict demand of environmental protection policy, traditional pyrogenic process proposes antimony technique and does not adapt to now
Some environmental protection policies.In addition, a large amount of exploitations and smelting of stibnite resource, cause low-grade stibnite resource to increase, these product
The low raw material in position is not able to satisfy the requirement of pyrogenic attack.And wet processing processing is for handling low-grade stibnite and eliminating low dense
Spend SO2Pollution have apparent advantage.In this background, numerous scientific workers fall back on mentions in the new wet process of exploitation
Antimony technique is taken, and achieves certain achievement.At present the technique of wet underwater welding antimony mainly have vulcanized sodium leaching-diaphragm electrodeposition method,
New chloride-hydrolysis, villaumite chlorination-low temperature distillation method, chlorine gas selecting lixiviation process, ozone leaching-Hydrolyze method etc..These methods
Solves SO2Pollution problem to environment, realizes the separation of lead, antimony, but there is also such as intermediate product accumulating amounts big, equipment
The problems such as seriously corroded, poor apparatus adaptability.Therefore it is sharp for the synthesis of antimony resource to develop a kind of new stibium by wet method extraction process
With being of great significance.
The reserves of China's pyrolusite are there are about 50,000,000 tons, wherein most of is low-grade lean ore.Currently, manganese resource
Dilution just restrict the production and sustainable development of China's manganese systems product.Pyrolusite is a kind of important manganese resource, existing
Pyrolusite reducing process technology can be divided into roasting method reduction and wet reducing two major classes.Disadvantage in roasting method reduction is equipment
It invests flue gas larger, that energy consumption is high, operating condition is poor, roasting process generates environment is caused seriously to pollute.Two-control region is China
Low-grade pyrolusite produces most common wet process route in manganese systems product process.However the shortcomings that two-control region is reduction rate
With leaching rate is lower, the quantity of slag is big, affect the rate of recovery of manganese, therefore find suitable reducing agent participation there is synthetical recovery manganese
Important meaning.
Summary of the invention
For described problem existing for this field, simple, work that an object of the present invention is to provide a kind of technological operations
Skill condition requires the method that low, clean and environmental protection, energy while Leaching of Antimony manganese, antimony manganese leaching rate are high and are easily isolated antimony manganese.
Realize the technical solution of the object of the invention are as follows:
A method of from Leaching of Antimony manganese simultaneously in stibnite and pyrolusite, comprising steps of
1) stibnite is placed in hydrochloric acid solution with pyrolusite and is leached simultaneously, then will leached ore pulp progress liquid and divide admittedly
From obtaining the leachate I and sulfur-bearing leached mud containing antimony manganese salt solution；
2) add antimony powder reduction into leachate I, obtain the leachate II based on antimony trichloride and manganese chloride,
3) leachate II is hydrolyzed, and can get antimony oxychloride hydrolysis residue and manganese chloride solution after solid-liquor separation.
The technological principle of above-mentioned technical proposal of the present invention are as follows: using stibnite and pyrolusite as raw material, technical hydrochloric acid is to leach
Agent, in leaching process, the iron in mine plays the effect of catalyst, and it is anti-that redox occurs in hydrochloric acid medium for stibnite and pyrolusite
It answers, antimony manganese enters ore pulp with ionic forms, and sulphur enters ore pulp in the form of elemental sulfur, and the leachate I after solid-liquor separation uses antimony
Powder reduction, obtains the leachate II based on antimony trichloride and manganese chloride, then leachate II is hydrolyzed, after solid-liquor separation
It can be obtained antimony oxychloride hydrolysis residue and manganese chloride solution.The key reaction occurred in whole process are as follows:
Sb2S3+4MnO2+ 16HCl=SbCl3+SbCl5+4MnCl2+3S+8H2O
2Sb+3SbCl5=5SbCl3
4SbCl3+5H2O=Sb4O5Cl2+10HCl
Stibnite is a kind of good reducing agent, and the electronic structure and ingredient of mineral are very suitable for MnO2Reduction；
In addition, antimony is also easy to separate with manganese and other impurity in leachate.This method carries out pyrolusite using stibnite as reducing agent
It leaches, this new process not only contributes to the promoter manganese in synthetical recovery manganese ore, while practicable also for low-grade antimony resource
Effective synthetical recovery realizes the short route of calcium halophosphate activated by antimony andmanganese clean manufacturing.
Further, in the stibnite mass fraction containing antimony be 35%~60%, and the primary chemical in stibnite at
It is divided into Sb2S3, the pyrolusite is containing MnO2Mass fraction be 30%~50%；The mixing of stibnite and pyrolusite in step 1)
Mn/S moles is 0.5/1~2/1 in ore pulp.
The selection and optimization of granularity are for guaranteeing that the normal leaching of mineral is of great significance with energy-saving.The present invention
In, the granularity of stibnite and pyrolusite is 180~250 mesh independently of each other in step 1)；The initial concentration of the hydrochloric acid solution
For 3mol/L~6mol/L.
Wherein, in step 1), control liquid-solid ratio (mL/g) is 3/1~10/1, in leaching process temperature control 50 DEG C~
95 DEG C, extraction time control is 2h~5h.
Improving extraction temperature can be improved the leaching rate of antimony, but the excessively high hydrochloric acid of temperature is easy to volatilize, and reduces leaching rate instead, and
It will increase task difficulty.Therefore preferably it is rapid 1) in, control liquid-solid ratio (mL/g) is 5/1~10/1, temperature control in leaching process
At 70 DEG C~90 DEG C.
Wherein, it is stirred when step 1) leaches, mixing speed is 300~600r/min.
Wherein, step 1) will leach ore pulp at a temperature of for 50 DEG C~95 DEG C and be filtered.
The method of Leaching of Antimony manganese simultaneously in above-mentioned slave stibnite and pyrolusite, it is preferred that after the leaching process
Obtained ore pulp is separated by solid-liquid separation under the extraction temperature.While hot filtering be consider heating pulp slurry be easier to filter, and
Solubility is bigger at high temperature for antimony, and when cooling, the antimony dissolved may be precipitated, hence into the recycling in slag, influencing antimony
Rate.
Wherein, in step 2), in reducing leaching liquid I be added antimony powder amount be solution in antimony theory total amount (mole) 1~
1.5 times, after reacting 0.5~2h, with the method separation leachate II and excessive antimony powder of suction filtration, gained antimony powder is returned again after filtering
It uses.
Wherein, in step 3), one of water, sodium carbonate, sodium bicarbonate, ammonium hydroxide or a variety of, control are added into leachate II
The pH value 0.1~0.4 of leachate II processed, to ensure that antimony is fully hydrolyzed.
The beneficial effects of the present invention are:
Present invention Leaching of Antimony manganese simultaneously from stibnite and pyrolusite using wet processing, effectively prevents pyrometallurgical smelting mistake
The problems such as production environment is poor in journey, sulfur dioxide pollution is serious.This method is suitable for low-grade stibnite and pyrolusite, to mention
The high increasingly utilization rate of the antimony ore and manganese resource of dilution reduces environmental pollution.
The technology that the present invention uses, which is compared with the traditional method, has the advantage that stibnite and pyrolusite in hydrochloric acid medium
Directly leach simultaneously, by the techniques such as leading reduction roasting acidleach roasting and leaching etc. concentrate on during acidleach completing,
And through subsequent reduction and purified treatment, separate antimony manganese.Finally simplify process flow, equipment is reduced, process intensification,
Realize that stibnite is efficiently leached and separated simultaneously with the antimony manganese in pyrolusite.
On the whole, technological operation of the invention is simple, and process conditions require low, clean and environmental protection, and antimony manganese leaching rate is high, money
Source comprehensive utilization degree is high, is a kind of very simple and effective hydrometallurgy of Leaching of Antimony manganese simultaneously from stibnite and pyrolusite
Method.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is the present invention
Some embodiments for those of ordinary skill in the art without creative efforts, can also basis
These attached drawings obtain other attached drawings.
Fig. 1 is the process flow chart of the method for the present invention.
Fig. 2 is the SEM-EDS figure of leached mud in embodiment 1 in the method for the present invention.
Fig. 3 is the XRD diagram of leached mud in embodiment 1 in the method for the present invention.
Fig. 4 is the SEM-EDS figure of leached mud in embodiment 3 in the method for the present invention.
Fig. 5 is the XRD diagram of leached mud in embodiment 3 in the method for the present invention.
Specific embodiment
The present invention is now illustrated with following most preferred embodiment, but is not intended to limit the scope of the invention.
The specific embodiment of the method for Leaching of Antimony manganese simultaneously in slave stibnite of the invention and pyrolusite, generally comprise with
Lower implementation steps:
(1) stibnite for being 35%~60% with mass fraction containing antimony and mass fraction containing manganese dioxide is 30%~50%
Pyrolusite be raw material, and the main compound ingredient in stibnite is Sb2S3, and the main compound ingredient in pyrolusite is
MnO2。
(2) hydrochloric acid for preparing 3mol/L~6mol/L, is heated to 50 DEG C~90 DEG C for hydrochloric acid, by particle size range 180~
The above-mentioned stibnite of 250 purposes and pyrolusite are added in the reactive tank for being loaded with hydrochloric acid, are controlled pulp slurry in leaching process and are compared admittedly
It (mL/g) is 3/1~10/1, ore pulp is sufficiently stirred in mixing speed control in 300~600r/min, leaching process, makes stibnite
It is evenly distributed and comes into full contact in hydrochloric acid medium with pyrolusite, maintain mixing time 2h~5h under normal pressure.
(3) ore pulp obtained after leaching process carries out separation of solid and liquid filtering while hot under extraction temperature, obtains with chlorine
The slag phase changing the leachate I based on antimony and manganese chloride and being made of elemental sulfur and other gangues.
(4) the antimony powder reducing leaching liquid I for being 1~1.5 with excess coefficient obtains the leaching based on antimony trichloride and manganese chloride
Liquid II out, extra antimony powder return continue to use.
(5) add water or sodium carbonate or sodium bicarbonate or ammonium hydroxide into leachate II, the pH of control leachate II is not less than
0.1, it is fully hydrolyzed antimony trichloride, antimony oxychloride hydrolysis residue and manganese chloride solution are obtained after solid-liquor separation.
To facilitate the understanding of the present invention, the present invention is made below in conjunction with Figure of description and preferred embodiment more complete
Face meticulously describes, but the protection scope of the present invention is not limited to the following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can be in markets
On be commercially available or be prepared through existing method.
Embodiment 1:
A method of the Leaching of Antimony manganese of the invention simultaneously from stibnite and pyrolusite as shown in Figure 1, specifically include with
Lower step:
(1) stibnite for being 42% with mass fraction containing antimony contains MnO2The pyrolusite of mass fraction 38.18% is raw material,
The main component of stibnite is Sb2S3。
(2) the hydrochloric acid 500mL for configuring 4mol/L, is heated to 70 degree for hydrochloric acid, by the partial size being crushed 180~250
Mesh stibnite and pyrolusite are raw material, are added in the reactive tank for filling hydrochloric acid after weighing well according to Mn/S (molar ratio) 1.2/1,
Hydrochloric acid volume is 5/1 measurement according to liquid-solid ratio (mL/g).Stirring is uniformly distributed stibnite and pyrolusite in hydrochloric acid simultaneously sufficiently
Reaction.
(3) revolving speed 400r/min, extraction time 2h are controlled in leaching process.
(4) ore pulp obtained after leaching process is filtered while hot under extraction temperature, is obtained with antimony chloride and chlorine
The slag phase changing the solution based on manganese and being made of elemental sulfur and other gangues.
The SEM-EDS figure of its slag is as shown in Figure 2.XRD spectrum is as shown in Figure 3.It is known in leachate I by detection with chlorination
Based on antimony and manganese chloride, sulfur-bearing slag phase is mainly made of elemental sulfur and other gangues.Through detecting, the leaching of metallic antimony in the present embodiment
Extracting rate is 86%, and the leaching rate of manganese metal is greater than 99%.
(5) antimony powder that excess coefficient is 1 of leachate I is restored, nutsch filter solid-liquor separation is used after 1 hour, is obtained with three
Leachate II based on antimony chloride and manganese chloride adds water and sodium bicarbonate into leachate II, monitors leachate II with pH meter
PH be 0.1, be fully hydrolyzed antimony trichloride, up to antimony oxychloride hydrolysis residue and manganese chloride solution after solid-liquor separation, realize antimony manganese
Separation measures antimony ion concentration in manganese chloride solution with ICP and is lower than 10mg/L.
Embodiment 2:
(1) stibnite for being 42% with mass fraction containing antimony contains MnO2The pyrolusite of mass fraction 38.18% is raw material,
The main component of stibnite is Sb2S3。
(2) the hydrochloric acid 500mL for configuring 5mol/L, is heated to 80 degree for hydrochloric acid, by the partial size being crushed 180~250
Mesh is to be added in the reactive tank for filling hydrochloric acid after 1.2/1 weighing is good according to Mn/S (mole), and hydrochloric acid volume is according to liquid-solid ratio
(mL/g) it is measured for 7/1.Stirring is uniformly distributed stibnite in hydrochloric acid with pyrolusite and sufficiently reacts.
(3) revolving speed 500r/min, extraction time 4h are controlled in leaching process.
(4) ore pulp obtained after leaching process is filtered while hot under extraction temperature, is obtained with antimony chloride and chlorine
The slag phase changing the solution based on manganese and being made of elemental sulfur and other gangues.
Through detecting, the leaching rate of metallic antimony is 92.95% in the present embodiment, and the leaching rate of manganese metal is greater than 99%.
(5) to leachate I with excess coefficient be 1.2 antimony powder restore, after 1 hour with nutsch filter solid-liquor separation obtain with
Leachate II based on antimony trichloride and manganese chloride adds water and sodium carbonate into leachate II, monitors leachate II with pH meter
PH be 0.2, be fully hydrolyzed antimony trichloride, up to antimony oxychloride hydrolysis residue and manganese chloride solution after solid-liquor separation, realize antimony manganese
Separation measures antimony ion concentration in manganese chloride solution with ICP and is lower than 8mg/L.
Embodiment 3:
(1) stibnite for being 42% with mass fraction containing antimony contains MnO2The pyrolusite of mass fraction 38.18% is raw material,
The main component of stibnite is Sb2S3。
(2) the hydrochloric acid 500mL for configuring 5mol/L, is heated to 90 degree for hydrochloric acid, by the partial size being crushed 180~250
Mesh is to be added in the reactive tank for filling hydrochloric acid after 1.4/1 weighing is good according to Mn/S (mole), and hydrochloric acid volume is according to liquid-solid ratio
(mL/g) it is measured for 10/1.Stirring is uniformly distributed stibnite in hydrochloric acid with pyrolusite and sufficiently reacts.
(3) revolving speed 600r/min, extraction time 5h are controlled in leaching process.
(4) ore pulp obtained after leaching process is filtered while hot under extraction temperature, is obtained with antimony chloride and chlorine
The slag phase changing the solution based on manganese and being made of elemental sulfur and other gangues.The SEM-EDS figure of its slag is as shown in Figure 4.XRD spectrum
As shown in Figure 5.
Through detecting, the leaching rate of metallic antimony is 96.89% in the present embodiment, and the leaching rate of manganese metal is greater than 99%.
(6) antimony powder that excess coefficient is 1.4 of leachate I is restored, is obtained after 1 hour with nutsch filter solid-liquor separation with three
Leachate II based on antimony chloride and manganese chloride adds water or sodium carbonate or sodium bicarbonate or ammonium hydroxide into leachate II, uses pH meter
It monitors that the pH of leachate II is 0.3, is fully hydrolyzed antimony trichloride, up to antimony oxychloride hydrolysis residue and manganese chloride after solid-liquor separation
Solution realizes the separation of antimony manganese, measures antimony ion concentration in manganese chloride solution with ICP and is lower than 5mg/L.
Embodiment 4:
(1) stibnite for being 42% with mass fraction containing antimony contains MnO2The pyrolusite of mass fraction 38.18% is raw material,
The main component of stibnite is Sb2S3。
(2) the hydrochloric acid 500mL for configuring 4mol/L, is heated to 80 degree for hydrochloric acid, by the partial size being crushed 180~250
Mesh is to be added in the reactive tank for filling hydrochloric acid after 1.4/1 weighing is good according to Mn/S (mole), and hydrochloric acid volume is according to liquid-solid ratio
(mL/g) it is measured for 9/1.Stirring is uniformly distributed stibnite in hydrochloric acid with pyrolusite and sufficiently reacts.
(3) revolving speed 500r/min, extraction time 5h are controlled in leaching process.
(4) ore pulp obtained after leaching process is filtered while hot under extraction temperature, is obtained with antimony chloride and chlorine
The slag phase changing the solution based on manganese and being made of elemental sulfur and other gangues.
Through detecting, the leaching rate of metallic antimony is 96.28% in the present embodiment, and the leaching rate of manganese metal is greater than 99%.
(5) antimony powder that excess coefficient is 1.5 of leachate I is restored, is obtained after 1 hour with nutsch filter solid-liquor separation with three
Leachate II based on antimony chloride and manganese chloride adds water or sodium carbonate or sodium bicarbonate or ammonium hydroxide into leachate II, uses pH meter
It monitors that the pH of leachate II is 0.4, is fully hydrolyzed antimony trichloride, up to antimony oxychloride hydrolysis residue and manganese chloride after solid-liquor separation
Solution realizes the separation of antimony manganese, measures antimony ion concentration in manganese chloride solution with ICP and is lower than 3mg/L.
Above embodiment is only that preferred embodiments of the present invention will be described, is not carried out to the scope of the present invention
It limits, without departing from the spirit of the design of the present invention, this field ordinary engineering and technical personnel is to technical solution of the present invention
The all variations and modifications made, should fall within the scope of protection determined by the claims of the present invention.
Claims (7)
1. a kind of method of Leaching of Antimony manganese simultaneously from stibnite and pyrolusite, which is characterized in that comprising steps of
1) stibnite is placed in hydrochloric acid solution with pyrolusite and is leached simultaneously, then will leached ore pulp and carry out solid-liquor separation,
Obtain the leachate I and sulfur-bearing leached mud containing antimony manganese salt solution；Wherein, in the stibnite mass fraction containing antimony be 35%~
60%, and the main chemical compositions in stibnite are Sb2S3, the pyrolusite is containing MnO2Mass fraction be 30%~50%；Step
It is rapid 1) in the mixed ore pulp of stibnite and pyrolusite Mn/S moles be 0.5/1~2/1；
2) add antimony powder reduction into leachate I, obtain the leachate II based on antimony trichloride and manganese chloride；
3) leachate II is hydrolyzed: into leachate II plus water, sodium carbonate, sodium bicarbonate, two kinds in ammonium hydroxide, until leachate
II pH value is 0.1~0.4, to ensure that antimony is fully hydrolyzed；It can get antimony oxychloride hydrolysis residue and manganese chloride solution after solid-liquor separation.
2. the method according to claim 1, wherein the granularity of stibnite and pyrolusite is independent mutually in step 1)
Ground is 180~250 mesh；The initial concentration of the hydrochloric acid solution is 3mol/L~6mol/L.
3. method according to claim 1 or 2, which is characterized in that in step 1), control liquid-solid ratio (mL/g) be 3/1~
10/1, at 50 DEG C~95 DEG C, extraction time control is 2h~5h for temperature control in leaching process.
4. according to the method described in claim 3, it is characterized in that, control liquid-solid ratio (mL/g) is 5/1~10/ in step 1)
1, temperature control is at 70 DEG C~90 DEG C in leaching process.
5. method according to claim 1 or 2, which is characterized in that step 1) is stirred when leaching, and mixing speed is
300~600r/min.
6. method according to claim 1 or 2, which is characterized in that step 1) is that will leach at a temperature of 50 DEG C~95 DEG C
Ore pulp is filtered.
7. method according to claim 1 or 2, which is characterized in that in step 2), antimony powder is added in reducing leaching liquid I
Amount is 1~1.5 times of antimony theory total amount (mole) in solution, after reacting 0.5~2h, with the method separation leachate II of suction filtration with
Excessive antimony powder, the return of gained antimony powder reuses after filtering.
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