CN106744725A - The method that selenium is leached from cadmium selenide waste material - Google Patents
The method that selenium is leached from cadmium selenide waste material Download PDFInfo
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- CN106744725A CN106744725A CN201611175893.9A CN201611175893A CN106744725A CN 106744725 A CN106744725 A CN 106744725A CN 201611175893 A CN201611175893 A CN 201611175893A CN 106744725 A CN106744725 A CN 106744725A
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- Prior art keywords
- oxygen
- leaching
- alkali
- waste material
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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
- C01B19/008—Salts of oxyacids of selenium or tellurium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G11/00—Compounds of cadmium
Abstract
A kind of method the present invention relates to leach selenium in waste material from cadmium selenide, the method is using two sections of oxygen pressure alkali leachings, cadmium selenide waste material is first carried out into one section of oxygen pressure alkali leaching, the raw material that the leached mud of one section of oxygen pressure alkali leaching presses alkali to soak as two sections of oxygen, the leachate of two sections of oxygen pressure alkali leachings is back in one section of leaching agent of oxygen pressure alkali leaching；Wherein one section oxygen pressure alkali leaching and two sections of oxygen pressure alkali leachings are carried out in autoclave, and are passed through oxygen as oxidant.The method of the present invention, in the selenium in cadmium selenide waste material is present in leachate in the form of the sodium selenite completely, safety and environmental protection, selenium recovery is high, low cost.
Description
Technical field
A kind of method the invention belongs to leach selenium in field of hydrometallurgy, more particularly to waste material from cadmium selenide.
Background technology
Selenium is a kind of important dissipated metal, and its application field is related to electronics, glass, metallurgy, chemical industry, health care, agriculture
The fields such as industry.But content of the selenium in the earth's crust is only 0.05 ppm, and distribution dispersion, year supply it is limited.Therefore, from waste material
Reclaiming selenium has great economic worth.
Cadmium selenide（CdSe）Have at aspects such as photo resistance, solar cell, thin film transistor (TFT) and microwave amplifiers wide
General application.Substantial amounts of cadmium selenide waste material is produced during cadmium selenide production and processing and use, its selenium content is high, be to reclaim selenium weight
The source wanted.But still rarely have the report of recovery process in document.Trace sth. to its source, be acid leaching process, reaction is violent, and process is difficult
Control, is also easy to produce the H of severe toxicity2Se gases, without prospects for commercial application；And conventional alkali soaking technology is used, leaching effect is poor, and selenium is returned
Yield is low.
Therefore, it is necessary to provide a kind of new method that selenium is leached from cadmium selenide waste material.
The content of the invention
The present invention is in view of the shortcomings of the prior art or not enough, there is provided a kind of new side that selenium is leached from cadmium selenide waste material
Method, improves the rate of recovery of selenium, and selenium is reclaimed in the form of sodium selenite crystal.
To realize a kind of object defined above, the present invention leach selenium method in adopting the following technical scheme that waste material from cadmium selenide,
Characterized in that, press alkali to soak using two sections of oxygen, including：Cadmium selenide waste material is first carried out into one section of oxygen pressure alkali leaching, one section of oxygen pressure alkali leaching
Leached mud press the raw materials that alkali soak, the leachate of two sections of oxygen pressure alkali leachings to be back to one section of leaching agent of oxygen pressure alkali leaching as two sections of oxygen
In；
One section of oxygen pressure alkali leaching and two sections of oxygen pressure alkali leachings are carried out in autoclave, and are passed through oxygen as oxidation
Agent.
As a further improvement on the present invention, when one section of oxygen pressure alkali soaks in autoclave partial pressure of oxygen be 0.3 ~
0.5MPa；Partial pressure of oxygen is 0.8 ~ 1.2MPa in autoclave when two sections of oxygen pressure alkali soaks.
As a further improvement on the present invention, in the leaching agent of one section of oxygen pressure alkali leaching naoh concentration be 80 ~
120g/L；The leaching agent of two sections of oxygen pressure alkali leaching is the sodium hydroxide solution of 120 ~ 160g/L.
As a further improvement on the present invention, the leaching agent of one section of oxygen pressure alkali leaching also includes SeO3 2-And/or SeO4 2-
Ion.
As a further improvement on the present invention, the solid-to-liquid ratio of one section of oxygen pressure alkali leaching is 1：(4~6)；Two sections of oxygen pressures
The solid-to-liquid ratio of alkali leaching is 1：(4~6).
As a further improvement on the present invention, the extraction temperature of two sections of oxygen pressure alkali leaching is 120 ~ 180 DEG C.
As a further improvement on the present invention, two sections of oxygen pressure alkali soaks equal 2 ~ 4h of leaching.
As a further improvement on the present invention, after two sections of oxygen pressure alkali leaching terminates, circulating water is passed through, makes reaction
Temperature in the kettle is less than 60 DEG C.
As a further improvement on the present invention, Cd mass fractions are 58.7%, Se mass contents point in the cadmium selenide waste material
Number is 41.3%；The cadmium selenide waste material need to carry out broken sieving, control the granularity of cadmium selenide waste material to be not more than 0.15mm.
The present invention not only increases the leaching rate of selenium in cadmium selenide waste material, while by control using two sections of oxygen pressure alkali leachings
Partial pressure of oxygen when one section of oxygen pressure alkali soaks, in making the selenium in cadmium selenide waste material be present in leachate in the form of the sodium selenite completely.
The method that the present invention is provided, safety and environmental protection, selenium recovery is high, low cost.
Specific embodiment
Technical scheme is clearly and completely described below in conjunction with the embodiment of the present invention, it is clear that described implementation
Example is only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under the premise of creative work is not made, belongs to the model of present invention protection
Enclose.
The present invention is adopted the following technical scheme that：A kind of method that selenium is leached in waste material from cadmium selenide, it is characterised in that use
Two sections of oxygen pressure alkali leachings, including：
Cadmium selenide waste material is first carried out into one section of oxygen pressure alkali leaching, the original that one section of oxygen presses the leached mud of alkali leaching to press alkali to soak as two sections of oxygen
Material, the leachate of two sections of oxygen pressure alkali leachings is back in one section of leaching agent of oxygen pressure alkali leaching；
One section of oxygen pressure alkali leaching and two sections of oxygen pressure alkali leachings are carried out in autoclave, and are passed through oxygen as oxidation
Agent.
In the present invention, the form of cadmium selenide waste material may be bulk, sheet, granular, before oxygen pressure alkali soaks, first be crushed
Screening, the mesh number of the sieve for sieving at least is not less than 100 mesh, to control the granularity no more than 0.15mm of cadmium selenide waste material.
In the present invention, two sections of oxygen pressure alkali leaching leaching equipments used are autoclave, built-in stainless steel agitating paddle and cold
But water-circulating pipe.
It is 1 by solid-to-liquid ratio by the cadmium selenide waste material and the sodium hydroxide solution of 80 ~ 120g/L of crushing and screening in the present invention：
(4 ~ 6) are added in autoclave, open stirring, control mixing speed, after being warming up to 120 ~ 180 DEG C, start to be passed through oxygen,
Oxygen partial pressure in autoclave can not be too high, too high, and sodium selenite easily is further oxidized into sodium selenate, the present invention,
Preferably, partial pressure of oxygen control, in 0.3 ~ 0.5MPa, reacts 2 ~ 4h in autoclave, closes heating, is passed through recirculated cooling water, makes
Temperature is down to less than 60 DEG C in material in kettle, stops stirring, and feed liquid in kettle is filtered, obtain one section of oxygen pressure alkali leaching leached mud with
One section of oxygen pressure alkali leaching leachate.
In the present invention, one section of oxygen is pressed the sodium hydroxide solution of alkali leaching leached mud and 120 ~ 160g/L, be 1 by solid-to-liquid ratio：
(4 ~ 6), are added in autoclave, open stirring, after being warming up to 120 ~ 180 DEG C, are passed through oxygen, control the partial pressure of oxygen in kettle to be
0.8 ~ 1.2MPa, reacts 2 ~ 4h, closes heating, cooling, filtering.The partial pressure of oxygen of two sections of oxygen pressure alkali leaching and sodium hydroxide solution it is dense
Degree is apparently higher than one section of oxygen pressure alkali leaching, in order that the selenium complete oxidation in one section of oxygen pressure alkali phase analysis is leached, the two sections of oxygen pressures for obtaining
Alkali leaching leachate is back to during one section of oxygen pressure alkali soaks as leaching agent, and two sections of oxygen pressure alkali leaching leached muds are hydrogen-oxygen after washing drying
Cadmium crystal, recycles again.
In the present invention, the one section of oxygen pressure alkali leaching leachate that will be obtained can be directly used for evaporating, concentrating and crystallizing, obtain selenous acid
Sodium crystal.
The present invention presses alkali to soak by two sections of oxygen, and the selenium in cadmium selenide waste material is leached completely.Wherein, by controlling one section of oxygen
Partial pressure of oxygen when pressure alkali leaching is leached, it is to avoid the selenium over oxidation in cadmium selenide only makes selenium in the form of sodium selenite into sodium selenate
Into solution；Furthermore, two sections of oxygen pressure alkali leachings use partial pressure of oxygen and naoh concentration higher leaching agent higher, to ensure one
Selenium in section oxygen pressure alkali leaching leached mud is leached completely.The method that the present invention is provided, selenium is leached by from cadmium selenide waste material, selenium
Leaching rate is high, selenium, cadmium segregation ratio more thoroughly, with low cost, safety and environmental protection.
Raw material is cadmium selenide waste material in following examples, and wherein selenium mass fraction is 41.3%, and the mass fraction of cadmium is
58.7%。
Embodiment 1.
1）To adding 396g to cross the CdSe powder of 100 mesh sieves in 3L autoclaves, by liquid-solid ratio 6:1 adds 2376ml
Concentration is the liquid caustic soda solution of 80g/L, and closed reactor opens stirring, controls mixing speed 200r/min, after being warming up to 180 DEG C,
Start to be passed through oxygen, it is 0.3Mpa to control partial pressure of oxygen in kettle, and circulating water to room temperature is passed through after reaction 4h, and feed liquid in kettle is entered
Row filtering, obtains one section of oxygen pressure alkali leaching leached mud and one section of oxygen pressure alkali leaching leachate.
Wherein one section oxygen pressure alkali soaks the quality of leached mud（Dry weight）It is 353.6g, detects that wherein Se contents are through ICP-MS
25.3%, Cd content are 65.7%.
2）Press alkali leaching leached mud to be added in the autoclave of 3L one section of oxygen, be 4 by liquid-solid ratio:1 addition concentration be
The liquid caustic soda solution of 160g/L, after being warming up to 120 DEG C, is passed through oxygen, and it is 1.2Mpa to control partial pressure of oxygen in kettle, is passed through after reaction 2h and followed
Ring is water-cooled to 60 DEG C, and filtering, the two sections of oxygen pressure alkali leaching leachate for obtaining is back in one section of oxygen pressure alkali leaching leaching agent, two sections of oxygen
After pressure alkali leaching leached mud is through washing drying, quality is 306.0g, is 2.2%, Cd mass through ICP-MS detections wherein Se mass contents
Content is 75.7%.
In the present embodiment, two sections of total leaching rates of oxygen pressure alkali leaching Se are 0.34% for the total leaching rates of 95.8%, Cd.
Embodiment 2.
1）To the CdSe powder for adding 396g to cross after 100 mesh sieves in 3L autoclaves, by liquid-solid ratio 5:1, add
The naoh concentration of 1980ml is the leaching agent of 100g/L, and closed reactor opens stirring, control mixing speed 200r/
Min, after being warming up to 150 DEG C, starts to be passed through oxygen, and it is 0.5Mpa to control partial pressure of oxygen in kettle, and circulating water is passed through after reaction 4h
To 40 DEG C, feed liquid in kettle is filtered, obtained one section of oxygen pressure alkali leaching leached mud and one section of oxygen pressure alkali leaching leachate.
Wherein one section oxygen pressure alkali soaks the quality of leached mud（Dry weight）It is 350.4g, detects that wherein Se contents are through ICP-MS
23.9%, Cd content are 66.3%.
2）Press alkali leaching leached mud to be added in the autoclave of 3L one section of oxygen, be 6 by liquid-solid ratio:1, add concentration be
The liquid caustic soda solution of 120g/L, after being warming up to 150 DEG C, is passed through oxygen, and it is 1.0Mpa to control partial pressure of oxygen in kettle, is passed through after reaction 2h and followed
Ring is water-cooled to 50 DEG C, and filtering, the two sections of oxygen pressure alkali leaching leachate for obtaining is back in one section of oxygen pressure alkali leaching leaching agent, two sections of oxygen
After pressure alkali leaching leached mud is through washing drying, quality is 305.6g, is 1.9%, Cd mass through ICP-MS detections wherein Se mass contents
Content is 75.9%.
In the present embodiment, two sections of total leaching rates of oxygen pressure alkali leaching Se are 0.26% for the total leaching rates of 96.4%, Cd.
In the present embodiment, SeO is also included in one section of oxygen pressure alkali leaching leaching agent3 2-And SeO4 2-Ion.
Embodiment 3.
1）To the CdSe powder for adding 396g to cross after 100 mesh sieves in 3L autoclaves, by liquid-solid ratio 4:1, add
The naoh concentration of 1584ml is the leaching agent of 120g/L, and closed reactor opens stirring, control mixing speed 200r/
Min, after being warming up to 120 DEG C, starts to be passed through oxygen, and it is 0.5Mpa to control partial pressure of oxygen in kettle, and circulating water is passed through after reaction 4h
To 40 DEG C, feed liquid in kettle is filtered, obtained one section of oxygen pressure alkali leaching leached mud and one section of oxygen pressure alkali leaching leachate.
Wherein one section oxygen pressure alkali soaks the quality of leached mud（Dry weight）It is 355.2g, detects that wherein Se contents are through ICP-MS
26.0%, Cd content are 65.4%.
2）Press alkali leaching leached mud to be added in the autoclave of 3L one section of oxygen, be 5 by liquid-solid ratio:1, add concentration be
The liquid caustic soda solution of 140g/L, after being warming up to 180 DEG C, is passed through oxygen, and it is 1.2Mpa to control partial pressure of oxygen in kettle, is passed through after reaction 2h and followed
Ring is water-cooled to 50 DEG C, and filtering, the two sections of oxygen pressure alkali leaching leachate for obtaining is back in one section of oxygen pressure alkali leaching leaching agent, two sections of oxygen
After pressure alkali leaching leached mud is through washing drying, quality is 305.0g, is 1.7%, Cd mass through ICP-MS detections wherein Se mass contents
Content is 75.9%.
In the present embodiment, two sections of total leaching rates of oxygen pressure alkali leaching Se are 0.35% for the total leaching rates of 96.8%, Cd.
In the present embodiment, SeO is also included in one section of oxygen pressure alkali leaching leaching agent3 2-And SeO4 2-Ion.
In above example, the one section of oxygen pressure alkali leaching leachate for obtaining can be directly used for evaporating, concentrating and crystallizing, and recovery is obtained
Sodium selenite crystal, the two sections of oxygen pressure alkali leaching leached mud for obtaining is cadmium hydroxide crystal, can be used to reclaim cadmium.
The present invention presses alkali to soak by two sections of oxygen, and the selenium in cadmium selenide waste material is leached completely.Wherein, by controlling one section of oxygen
Partial pressure of oxygen when pressure alkali soaks, it is to avoid the selenium over oxidation in cadmium selenide only makes selenium enter in the form of sodium selenite into sodium selenate
Solution；Furthermore, two sections of oxygen pressure alkali leachings use partial pressure of oxygen and naoh concentration higher leaching agent higher, to ensure one section of oxygen
Selenium in pressure alkali leaching leached mud is leached completely.The method that the present invention is provided, by leaching selenium, the leaching of selenium from cadmium selenide waste material
Rate is high, and selenium and cadmium separative efficiency are high, with low cost, safety and environmental protection.
Although being example purpose, the preferred embodiment of the present invention, the ordinary skill people of this area are had been disclosed for
Member will be various to change, it is realized that in the case of scope and spirit of the present invention disclosed in not departing from by appending claims
It is possible for entering, increasing and replacing.
Claims (9)
1. a kind of method that selenium is leached in waste material from cadmium selenide, it is characterised in that using two sections of oxygen pressure alkali leachings, including：
Cadmium selenide waste material is first carried out into one section of oxygen pressure alkali leaching, the original that one section of oxygen presses the leached mud of alkali leaching to press alkali to soak as two sections of oxygen
Material, the leachate of two sections of oxygen pressure alkali leachings is back in one section of leaching agent of oxygen pressure alkali leaching；
One section of oxygen pressure alkali leaching and two sections of oxygen pressure alkali leachings are carried out in autoclave, and are passed through oxygen as oxidation
Agent.
2. the method that selenium is leached in the waste material from cadmium selenide according to claim 1, it is characterised in that one section of oxygen presses alkali
Partial pressure of oxygen is 0.3 ~ 0.5MPa in autoclave during leaching；When two sections of oxygen pressure alkali soaks in autoclave partial pressure of oxygen be 0.8 ~
1.2MPa。
3. the method that selenium is leached in the waste material from cadmium selenide according to claim 1, it is characterised in that one section of oxygen presses alkali
Naoh concentration is 80 ~ 120g/L in the leaching agent of leaching；The leaching agent of two sections of oxygen pressure alkali leaching is the hydrogen of 120 ~ 160g/L
Sodium hydroxide solution.
4. the method that selenium is leached in the waste material from cadmium selenide according to claim 1, it is characterised in that one section of oxygen presses alkali
The leaching agent of leaching also includes SeO3 2-And/or SeO4 2-Ion.
5. the method that selenium is leached in the waste material from cadmium selenide according to claim 3, it is characterised in that one section of oxygen presses alkali
The solid-to-liquid ratio of leaching is 1：(4~6)；The solid-to-liquid ratio of two sections of oxygen pressure alkali leaching is 1：(4~6).
6. the method that selenium is leached in the waste material from cadmium selenide according to claim 1, it is characterised in that two sections of oxygen presses alkali
The extraction temperature of leaching is 120 ~ 180 DEG C.
7. the method that selenium is leached in the waste material from cadmium selenide according to claim 1, it is characterised in that two sections of oxygen presses alkali
Soak equal 2 ~ 4h of leaching.
8. the method that selenium is leached in the waste material from cadmium selenide according to claim 1, it is characterised in that two sections of oxygen presses alkali
After leaching terminates, circulating water is passed through, reactor temperature is less than 60 DEG C.
9. according to any described method that selenium is leached from cadmium selenide waste material of claim 1 ~ 8, it is characterised in that the selenizing
Cd mass fractions are that 58.7%, Se mass contents fraction is 41.3% in cadmium waste material；The cadmium selenide waste material need to carry out broken sieving,
The granularity of cadmium selenide waste material is controlled to be not more than 0.15mm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112125286A (en) * | 2020-09-18 | 2020-12-25 | 先导薄膜材料（广东）有限公司 | Arsenic or compound thereof doped cadmium selenide and preparation method thereof, thin film solar cell and preparation method thereof |
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| CN112125286A (en) * | 2020-09-18 | 2020-12-25 | 先导薄膜材料（广东）有限公司 | Arsenic or compound thereof doped cadmium selenide and preparation method thereof, thin film solar cell and preparation method thereof |
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