CN110255509A - A kind of technique for producing tellurium dioxide - Google Patents
A kind of technique for producing tellurium dioxide Download PDFInfo
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- CN110255509A CN110255509A CN201910660913.9A CN201910660913A CN110255509A CN 110255509 A CN110255509 A CN 110255509A CN 201910660913 A CN201910660913 A CN 201910660913A CN 110255509 A CN110255509 A CN 110255509A
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- tellurium
- copper
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/004—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The present invention provides a kind of techniques for producing tellurium dioxide, comprising the following steps: A) mixed acid reaction will be added after tellurium copper slurry, obtain pre- leaching slurry；B) pH to 2~4 will be adjusted after the pre- leaching slurry and oxidant reaction, obtains high copper liquid and rich tellurium slag；C it) will be reacted after the rich tellurium slurry with transition agent, removing impurities agent, obtain transition slurries；The transition slurries and alkali are reacted, point tellurium tailings and tellurium leachate are obtained；D) the tellurium leachate is hydrolyzed, obtains tellurium dioxide.Present invention firstly provides presoak decopper(ing) by control weakly acidic condition, reoxidize autoprecipitation tellurium, tellurium copper is efficiently separated, then transition agent and removing impurities agent imurity-removal and transition high price tellurium are added before soaking by alkali, the processing step realizes multi-functional under the conditions of brief, easily controllable, and makes leaching rate height, removing impurities effect is good, and the copper tellurium rate of recovery is high.
Description
Technical field
The present invention relates to minor metals recovery technology field more particularly to a kind of techniques for producing tellurium dioxide.
Background technique
Tellurium metal content is rare, but uses extensively in certain specific areas, such as: the cooling and warming of solar battery, stone
The catalyst of oily cracking, the brightener of electroplate liquid, the coloured material of glass, to increase the additive of steel ductility, to increase
The intensity of leading and corrosion proof additive, further, tellurium and its compound are a kind of semiconductor material again.Though as a result,
The content of right tellurium is rare, but it is widely used, and therefore, the demand of tellurium is still very big.
The extraction source of tellurium is mainly in copper anode mud and waste material containing tellurium；Industrial application is more for copper powder displacement at present
Then tellurium copper slag is carried out acid Strong oxdiative leaches, alkali soaks or high pressure leaches etc. at tellurium copper slag by tellurium.Copper in acid Strong oxdiative liquid
Be difficult to separate with tellurium, using oxalic acid decopper(ing) but at high cost, filtration difficulty, and Strong oxdiative leach in tellurium valence state ingredient it is multiple
Miscellaneous, the rate of recovery is not high, and loss is big；Leaching rate is low when alkaline leaching, and there are a large amount of peroxidating or the incomplete situations of oxidation, and
And the alkali phase analysis cupric quantity of slag is big, especially high copper ashes the case where, filtration difficulty is inconvenient；There are equipment investments for high pressure leaching
Height, easy peroxidating situation, and equipment cost investment is big, the bad adaptability of more materials.
Based on the above circumstances, it is desirable to provide the new technique of one kind is carried out with low cost, the efficient tellurium in tellurium copper slag
Recycling.
Summary of the invention
Present invention solves the technical problem that being to provide a kind of technique for producing tellurium dioxide, technique provided by the present application is certainly
Tellurium dioxide is produced in tellurium copper slag, keeps the rate of recovery of tellurium dioxide and purity higher.
In view of this, this application provides a kind of techniques for producing tellurium dioxide, comprising the following steps:
A) mixed acid reaction will be added after tellurium copper slurry, obtains pre- leaching slurry；The mixed acid is sulfuric acid and hydrochloric acid；
B) pH to 2~4 will be adjusted after the pre- leaching slurry and oxidant reaction, obtains high copper liquid and rich tellurium slag；
C it) will be reacted after the rich tellurium slurry with transition agent, removing impurities agent, obtain transition slurries；By the transition slurries and
Alkali reaction, obtains point tellurium tailings and tellurium leachate；
D) the tellurium leachate is hydrolyzed, obtains tellurium dioxide.
Preferably, the content of tellurium is greater than 10wt% in the tellurium copper slag, and the content of copper is less than 60wt%.
Preferably, the molar ratio of the mixed acid and the tellurium copper slag is 1:(1~2), the concentration of hydrochloric acid is 5~10g/
L.(restriction of mixed acid defines in claim 1)
Preferably, step A) in, the solid-to-liquid ratio of tellurium copper slag and water described in the pulp is 4~10, the temperature of the reaction
Degree is 70~90 DEG C, and the time of the reaction is 15~30min.
Preferably, step B) described in oxidant be hydrogen peroxide, chlorine, sodium chlorate, potassium chlorate, perchloric acid and sodium hypochlorite
One of or it is a variety of；The time of the reaction is 1~2h.
Preferably, step C) in, the transition agent is one of sodium sulfite, sodium pyrosulfite and sulfur dioxide or more
Kind, the removing impurities agent is one of hydrochloric acid, sodium chloride and potassium chloride or a variety of；It is described transition agent be the tellurium copper slag 1~
5wt%, the removing impurities agent are 1~5wt% of the tellurium copper slag；The solid-to-liquid ratio of richness tellurium slag and water described in the pulp be 4~
10；The additional amount of the alkali is 20~40wt% of the tellurium copper slag.
Preferably, step C) in, temperature react with transition agent, removing impurities agent is 70~90 DEG C, the time for 0.5~
1h；The temperature of described and alkali reaction is 70~90 DEG C, and the time is 1~2h.
Preferably, the reagent that the hydrolysis is added is the diluted sulfuric acid of 1:1.
Preferably, the temperature of the hydrolysis is 70~80 DEG C, and the time is 0.5~1h, and the terminal pH of the hydrolysis is 5~6.
This application provides a kind of techniques for producing tellurium dioxide, will presoak in mixed acid after tellurium copper slurry first
Decopper(ing) is added oxidant and guarantees that tellurium copper slag can be leached effectively, and high-valence state tellurium occurs in maximum possible inhibition, by controlling oxygen
PH after changing reaction ensure that tellurium and copper efficiently separate, and add transition agent, removing impurities agent ensure that remaining high price tellurium in rich tellurium slag
It is reduced, greatly improves the rate of recovery of tellurium in alkali leaching process, and impurity element is effectively restored, finally obtained dioxy
Change tellurium, the experimental results showed that, the rate of recovery of tellurium is up to 98%, and the purity of tellurium dioxide is up to 99%.
Detailed description of the invention
Fig. 1 is that tellurium produces flow diagram in tellurium copper slag of the present invention.
Specific embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described below with reference to embodiment, still
It should be appreciated that these descriptions are only further explanation the features and advantages of the present invention, rather than to the claims in the present invention
Limitation.
In view of the problem of tellurium copper slag produces tellurium dioxide in the prior art, the embodiment of the invention discloses one kind to produce dioxy
The technique for changing tellurium, the technique can efficiently separate copper, the tellurium in tellurium copper slag, and in the case where controlling low cost, greatly
Improve the rate of recovery of tellurium；The application produces the process flow diagram of tellurium dioxide as shown in Figure 1, comprising: pre- decopper(ing)-oxidation
It drowns oneself tellurium-transition, removal of impurities-alkali leaching-hydrolysis-tellurium dioxide；More specifically, the technique for producing tellurium dioxide, including it is following
Step:
A) mixed acid reaction will be added after tellurium copper slurry, obtains pre- leaching slurry；The mixed acid is sulfuric acid and hydrochloric acid；
B) pH to 2~4 will be adjusted after the pre- leaching slurry and oxidant reaction, obtains high copper liquid and rich tellurium slag；
C it) will be reacted after the rich tellurium slurry with transition agent, removing impurities agent, obtain transition slurries；By the transition slurries and
Alkali reaction, obtains point tellurium tailings and tellurium leachate；
D) the tellurium leachate is hydrolyzed, obtains tellurium dioxide.
During producing tellurium dioxide, the application by tellurium copper slurry, obtains tellurium copper dreg slurry first, adds mixed
Acid reaction is closed to get pre- leaching slurry is arrived；In the process, mixed acid inhibits oxidation autoreduction to efficiently separate copper tellurium, high tellurium
The quantity of slag is greatly reduced, and ensure that the preferential progress of alkali leaching, reduces time and the cost of filtering, and the mixed acid is sulfuric acid and salt
Acid, wherein hydrochloric acid plays the role of inhibition, and the tellurium of high price is reduced into low price tellurium as inhibitor, ensure that in oxidant condition
The generation of lower control high price tellurium, ensure that the leaching rate of tellurium；The reduction process of tellurium has chlorine generation simultaneously, becomes again in liquid
Oxidant continues tellurium oxide copper ashes, plays the role of circulation and promotes, simultaneously because have acid group in hydrochloric acid, the addition supplemented with acid.
The solid-to-liquid ratio of tellurium copper slag and water described in herein described pulp is 4~10；The molar ratio of the mixed acid and the tellurium copper slag
For 1:(1~2), the concentration of the hydrochloric acid is 5~10g/L；The sulfuric acid and the chlorhydria can make liquid acidity high, impurity
More enter solution, but tellurium can be also partly dissolved in liquid, keep the rate of recovery of tellurium poor, but few then acid was added not in mixed acid
It is enough, react insufficient, so that tellurium leaching rate is low.The temperature of above-mentioned premixing acid reaction is 70~90 DEG C, the time of the reaction
For 15~30min.
According to the present invention, pH to 2~4 will be adjusted after the pre- leaching slurry and oxidant reaction then to get high-copper is arrived
Liquid and rich tellurium slag；The process, which passes through oxidant and leaches and control pH, ensure that tellurium in tellurium copper slag, copper efficiently separate.The oxidation
Agent is chosen in particular from one of hydrogen peroxide, chlorine, sodium chlorate, potassium chlorate, perchloric acid and hypochlorous acid or a variety of, in specific embodiment
In, the oxidant is selected from chlorine.The pH value is too small, then the acidity of slurries is high, and tetravalence tellurium and few sexavalence tellurium all can be molten
Solution, the tellurium rate of recovery is low, and pH is excessive, and acidity is low, reacts insufficient.The time of the reaction is 1~2h.High-copper obtained above
Liquid then neutralizes outlet.
Then the application will react after the rich tellurium slurry with transition agent, removing impurities agent, by remaining height in rich tellurium slag
Valence tellurium is reduced, and impurity element is restored.The transition agent is in sodium sulfite, sodium pyrosulfite and sulfur dioxide
It is one or more, the removing impurities agent is one of hydrochloric acid, sodium chloride and potassium chloride or a variety of, in a particular embodiment, institute
It states transition agent and is selected from sulfur dioxide, the removing impurities agent is hydrochloric acid.The transition agent is 1~5wt% of the tellurium copper slag, described de-
Miscellaneous dose of 1~5wt% (or adjusting the pH of rich tellurium dreg slurry is 1~3) for the tellurium copper slag；Richness tellurium slag described in the pulp with
The solid-to-liquid ratio of water is 4~10.The temperature of above-mentioned reaction is 70~90 DEG C, and the time of reaction is 0.5~1h.
According to the present invention, then the transition slurries and alkali are reacted, tellurium leachate is obtained and divides tellurium tailings, wherein dividing tellurium
Tailings carries out melting processing；Transition, removing impurities technique before alkali leaching ensure that remaining high price tellurium is reduced in rich tellurium slag, then can be
The rate of recovery is greatly improved in alkali leaching process.In the process, the alkali is selected from piece alkali, and additional amount is the 20~40% of tellurium copper slag.
The temperature of above-mentioned reaction is 70~90 DEG C, and the time is 1~2h.
The application finally the tellurium leachate is hydrolyzed to get tellurium dioxide is arrived；The hydrolysis is soaked in the tellurium
The diluted sulphuric acid hydrolysis of 1:1 is added in liquid out, control terminal pH is 5~6,70~80 DEG C of temperature, reacts 0.5~1h.Above-mentioned water
Tellurium is purified by control pH and the further imurity-removal of temperature, has obtained purer tellurium dioxide by solution.
This application provides a kind of techniques that tellurium dioxide is produced from tellurium copper slag comprising: pre- decopper(ing)-oxidation is drowned oneself
Tellurium-transition, removal of impurities-alkali leaching-a series of process of hydrolysis-tellurium dioxide, in the process, this technique is first with low acid-sulfuric acid
Oxidation autoreduction is inhibited to efficiently separate copper tellurium with hydrochloric acid, the high tellurium quantity of slag is greatly reduced, and ensure that effective progress of alkali leaching, is reduced
The time of filtering and cost；Hydrochloric acid ensure that the generation that high price tellurium is controlled under the conditions of oxidant as inhibitor, improve tellurium
Direct yield, while save acid use, do not introduce salt impurity；Leaching control pH by oxidant again ensure that copper tellurium
It efficiently separates, low acid inhibits the rate of recovery of tellurium oxide to reach 99.5%, and the removal efficiency of copper reaches 90%；Suppression is added before soaking operation in alkali
Removing impurities agent processed restores foreign matter selenium etc. under mild acid conditions, and high-valence state tellurium is reduced into lower valency, under the conditions of subsequent alkaline leaching
It improves tellurium leaching rate and reduces impurity content in alkali immersion liquid；Resulting tellurium leachate hydrolyzes operation, control pH and temperature into
One-step removal impurity further purifies tellurium, obtains purer tellurium dioxide and facilitates subsequent operation.
For a further understanding of the present invention, below with reference to embodiment to the technique provided by the invention for producing tellurium dioxide into
Row is described in detail, and protection scope of the present invention is not limited by the following examples.
Embodiment 1
200kg tellurium copper slag is taken, adds water with liquid according to liquid-solid ratio 6:1,93% sulfuric acid 65kg is added, hydrochloric acid 50kg is added, stirs
Reaction 15min is mixed, is passed through chlorine 50L/min to final control pH=3,75 DEG C of reaction temperature, reaction time 2h obtains high tellurium slag
120kg；
Add water with liquid according to liquid-solid ratio 6:1 high tellurium slag, is warming up to 75 DEG C, is passed through sulfur dioxide 30L/min, time
0.5h controls pH=1 by hydrochloric acid, piece alkali 75kg, reaction time 2h is then added, obtains a point tellurium tailings 23kg, tellurium leachate
843L；
Tellurium leachate is warming up to 70 DEG C, the diluted 93% sulfuric acid control of 1:1 is slowly added to pH=5~6, is obtained by filtration
Tellurium dioxide 87kg.
The data of raw material involved in above-mentioned preparation process and product are as shown in the table:
1 embodiment 1 of table produces the tables of data of raw material and product that tellurium dioxide is related to
By statistics, the removal efficiency of copper reaches 92.50%, and tellurium dioxide direct yield reaches 92.94%, divides tellurium tailings tellurium
5.18%, the rate of recovery of tellurium reaches 98.12%.
Embodiment 2
200kg tellurium copper slag is taken, adds water with liquid according to liquid-solid ratio 5:1,93% sulfuric acid 75kg is added, hydrochloric acid 44kg is added, stirs
Reaction 15min is mixed, is passed through chlorine 50L/min to final control pH=3,75 DEG C of reaction temperature, reaction time 2h obtains high tellurium slag
103kg；
High tellurium slag is matched into liquid according to liquid-solid ratio 6:1,75 DEG C is warming up to, is passed through sulfur dioxide 30L/min, time 0.5h, lead to
Persalt controls pH=1, and piece alkali 65kg, reaction time 2h is added, obtains a point tellurium tailings 15kg, tellurium leachate 742L；
Tellurium leachate is warming up to 70 DEG C, the diluted 93% sulfuric acid control of 1:1 is slowly added to pH=5~6, is obtained by filtration
Tellurium dioxide 68kg.
The data of raw material involved in above-mentioned preparation process and product are as shown in the table:
2 embodiment 2 of table produces the tables of data of raw material and product that tellurium dioxide is related to
By statistics, preferably, the removal efficiency of copper reaches 94.58% to the low tellurium material processing of high-copper, and tellurium dioxide direct yield reaches
94.13%, divide tellurium tailings tellurium 3.97%, the rate of recovery of tellurium reaches 98.17%.
Embodiment 3
200kg tellurium copper slag is taken, adds water with liquid according to liquid-solid ratio 6:1,93% sulfuric acid 67kg is added, hydrochloric acid 40kg is added, stirs
Reaction 15min is mixed, is passed through chlorine 50L/min to final control pH=3,75 DEG C of reaction temperature, reaction time 2h obtains high tellurium slag
132kg；
High tellurium slag is matched into liquid according to liquid-solid ratio 6:1,75 DEG C is warming up to, is passed through sulfur dioxide 30L/min, time 0.5h, lead to
Persalt controls pH=2, and piece alkali 75kg, reaction time 2h is added, obtains a point tellurium tailings 27kg, tellurium leachate 870L；
Tellurium leachate is warming up to 70 DEG C, the diluted 93% sulfuric acid control of 1:1 is slowly added to between pH=5~6, filters
Obtain tellurium dioxide 69kg.
The data of raw material involved in above-mentioned preparation process and product are as shown in the table:
3 embodiment 3 of table produces the tables of data of raw material and product that tellurium dioxide is related to
By statistics, preferably, the removal efficiency of copper reaches 92.24%, and tellurium dioxide direct yield reaches for high miscellaneous material processing
93.44%, divide tellurium tailings tellurium 4.82%, the rate of recovery of tellurium reaches 98.26%.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.It should be pointed out that pair
For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out
Some improvements and modifications, these improvements and modifications also fall within the scope of protection of the claims of the present invention.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (9)
1. a kind of technique for producing tellurium dioxide, comprising the following steps:
A) mixed acid reaction will be added after tellurium copper slurry, obtains pre- leaching slurry；The mixed acid is sulfuric acid and hydrochloric acid；
B) pH to 2~4 will be adjusted after the pre- leaching slurry and oxidant reaction, obtains high copper liquid and rich tellurium slag；
C it) will be reacted after the rich tellurium slurry with transition agent, removing impurities agent, obtain transition slurries；The transition slurries and alkali are anti-
It answers, obtains point tellurium tailings and tellurium leachate；
D) the tellurium leachate is hydrolyzed, obtains tellurium dioxide.
2. technique according to claim 1, which is characterized in that the content of tellurium is greater than 10wt% in the tellurium copper slag, copper
Content is less than 60wt%.
3. technique according to claim 1, which is characterized in that the molar ratio of the mixed acid and the tellurium copper slag is 1:(1
~2), the concentration of hydrochloric acid is 5~10g/L.
4. technique according to claim 1, which is characterized in that step A) in, tellurium copper slag described in the pulp and water
Solid-to-liquid ratio is 4~10, and the temperature of the reaction is 70~90 DEG C, and the time of the reaction is 15~30min.
5. technique according to claim 1, which is characterized in that step B) described in oxidant be hydrogen peroxide, chlorine, chloric acid
One of sodium, potassium chlorate, perchloric acid and sodium hypochlorite are a variety of；The time of the reaction is 1~2h.
6. technique according to claim 1, which is characterized in that step C) in, the transition agent is sodium sulfite, burnt sulfurous
One of sour sodium and sulfur dioxide are a variety of, and the removing impurities agent is one of hydrochloric acid, sodium chloride and potassium chloride or a variety of；Institute
1~5wt% that transition agent is the tellurium copper slag is stated, the removing impurities agent is 1~5wt% of the tellurium copper slag；Institute in the pulp
The solid-to-liquid ratio for stating rich tellurium slag and water is 4~10；The additional amount of the alkali is 20~40wt% of the tellurium copper slag.
7. technique according to claim 1, which is characterized in that step C) in, the temperature reacted with transition agent, removing impurities agent
Degree is 70~90 DEG C, and the time is 0.5~1h；The temperature of described and alkali reaction is 70~90 DEG C, and the time is 1~2h.
8. technique according to claim 1, which is characterized in that the reagent that the hydrolysis is added is the diluted sulfuric acid of 1:1.
9. technique according to claim 8, which is characterized in that the temperature of the hydrolysis be 70~80 DEG C, the time be 0.5~
1h, the terminal pH of the hydrolysis are 5~6.
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| CN112695199A (en) * | 2020-12-15 | 2021-04-23 | 广东先导稀贵金属材料有限公司 | Method for extracting tellurium and copper from tellurium-copper slag |
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| CN110255509B (en) | 2021-02-12 |
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