CN106744725B - 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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- CN106744725B CN106744725B CN201611175893.9A CN201611175893A CN106744725B CN 106744725 B CN106744725 B CN 106744725B CN 201611175893 A CN201611175893 A CN 201611175893A CN 106744725 B CN106744725 B CN 106744725B
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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
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Abstract
The present invention relates to a kind of methods that selenium is leached in waste material from cadmium selenide, this method presses alkali leaching using two sections of oxygen, cadmium selenide waste material is first subjected to one section of oxygen pressure alkali leaching, the leachate of raw material of the leached mud of one section of oxygen pressure alkali leaching as two sections of oxygen pressure alkali leachings, two sections of oxygen pressure alkali leachings is back in the leaching agent of one section of oxygen pressure alkali leaching；Wherein one section of oxygen pressure alkali leaching and two sections of oxygen press alkali leaching to be carried out in autoclave, and are passed through oxygen as oxidant.The method of the present invention, makes the selenium in cadmium selenide waste material be present in leachate in the form of sodium selenite completely, safety and environmental protection, and selenium recovery is high, at low cost.
Description
Technical field
The invention belongs to the method for selenium is leached in field of hydrometallurgy more particularly to a kind of waste material from cadmium selenide.
Background technology
Selenium is a kind of important dissipated metal, and 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 be distributed dispersion, year supply it is limited.Therefore, from waste material
Recycling selenium has great economic value.
Cadmium selenide（CdSe）Have in photo resistance, solar cell, thin film transistor (TFT) and microwave amplifier etc. wide
General application.A large amount of cadmium selenide waste material is generated during cadmium selenide production and processing and use, selenium content is high, is recycling selenium weight
The source wanted.But still rarely has the report of recovery process in document.It traces sth. to its source, is acid leaching process, reaction is violent, and process is not easy
Control is also easy to produce the H of severe toxicity2Se gases, no prospects for commercial application；And conventional alkali soaking technology is used, leaching effect is poor, and selenium returns
Yield is low.
Therefore, it is necessary to a kind of method for leaching selenium in providing slave cadmium selenide waste material newly.
Invention content
The present invention is in view of the shortcomings of the prior art or insufficient, provides the side that selenium is leached in a kind of slave cadmium selenide waste material newly
Method improves the rate of recovery of selenium, and selenium is recycled in the form of sodium selenite crystal.
To realize that foregoing purpose, the present invention adopt the following technical scheme that a kind of method for leaching selenium in the waste material from cadmium selenide,
It is characterized in that, alkali leaching is pressed using two sections of oxygen, including：Cadmium selenide waste material is first subjected to one section of oxygen pressure alkali leaching, one section of oxygen pressure alkali leaching
Raw material of the leached mud as the pressure alkali leaching of two sections of oxygen, the leachate of two sections of oxygen pressure alkali leachings is back to the leaching agent of one section of oxygen pressure alkali leaching
In；
One section of oxygen pressure alkali leaching and two sections of oxygen press alkali leaching to be carried out in autoclave, and are passed through oxygen as oxygen
Agent.
As a further improvement on the present invention, when the leaching of one section of oxygen pressure alkali 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 leaching.
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 sodium hydroxide solution that the leaching agent of two sections of oxygen pressure alkali leaching is 120 ~ 160g/L.
As a further improvement on the present invention, the leaching agent of one section of oxygen pressure alkali leaching further 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, it is passed through circulating water, 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, and the granularity of control cadmium selenide waste material is not more than 0.15mm.
The present invention presses alkali leaching using two sections of oxygen, not only increases the leaching rate of selenium in cadmium selenide waste material, while passing through control
Partial pressure of oxygen when one section of oxygen pressure alkali leaching, makes the selenium in cadmium selenide waste material be present in leachate in the form of sodium selenite completely.
Method provided by the invention, safety and environmental protection, selenium recovery is high, at low cost.
Specific implementation mode
Technical solution 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 the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
The every other embodiment that technical staff is obtained without making creative work belongs to the model that the present invention protects
It encloses.
The present invention adopts the following technical scheme that：A method of leaching selenium from cadmium selenide waste material, which is characterized in that use
Two sections of oxygen pressure alkali leachings, including：
Cadmium selenide waste material, which is first carried out one section of oxygen, presses alkali leaching, the leached mud that one section of oxygen pressure alkali soaks to be soaked as two sections of oxygen pressure alkali
The leachate of raw material, two sections of oxygen pressure alkali leachings is back in the leaching agent of one section of oxygen pressure alkali leaching；
One section of oxygen pressure alkali leaching and two sections of oxygen press alkali leaching to be carried out in autoclave, and are passed through oxygen as oxygen
Agent.
In the present invention, the form of cadmium selenide waste material may be bulk, sheet, granular, before oxygen pressure alkali soaks, be first crushed
The mesh number of screening, the sieve for screening is at least not less than 100 mesh, and the granularity to control cadmium selenide waste material is not more than 0.15mm.
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 of crushing and screening and the sodium hydroxide solution of 80 ~ 120g/L in the present invention：
(4 ~ 6) are added in autoclave, open stirring, are controlled mixing speed, after being warming up to 120 ~ 180 DEG C, are started to be passed through oxygen,
Oxygen partial pressure in autoclave cannot be too high, excessively high, is easy sodium selenite being further oxidized to sodium selenate, the present invention,
Preferably, partial pressure of oxygen control reacts 2 ~ 4h in 0.3 ~ 0.5MPa in autoclave, closes heating, is passed through recirculated cooling water, makes
Temperature is down to 60 DEG C hereinafter, stop stirring in material in kettle, and feed liquid in kettle is filtered, obtain one section of oxygen pressure alkali leaching leached mud and
One section of oxygen pressure alkali soaks leachate.
In the present invention, presses alkali to soak the sodium hydroxide solution of leached mud and 120 ~ 160g/L one section of oxygen, 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 partial pressure of oxygen in kettle and are
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 to make the selenium complete oxidation in one section of oxygen pressure alkali phase analysis leach, two sections of obtained oxygen pressures
Alkali leaching leachate is back in one section of oxygen pressure alkali leaching and is used as leaching agent, and two sections of oxygen pressure alkali leaching leached muds are hydrogen-oxygen after washing is dried
Cadmium crystal, recycles again.
In the present invention, presses alkali to soak leachate obtain one section of oxygen, can be directly used for evaporating, concentrating and crystallizing, obtain selenous acid
Sodium crystal.
The present invention presses alkali leaching 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 alkali leaching being pressed to leach, avoids the selenium excessive oxidation in cadmium selenide at sodium selenate, only makes selenium in the form of sodium selenite
Into solution；Furthermore two sections of oxygen pressure alkali leachings use higher partial pressure of oxygen and the higher leaching agent of naoh concentration, to ensure one
Selenium in section oxygen pressure alkali leaching leached mud leaches completely.Method provided by the invention, by leaching selenium from cadmium selenide waste material, selenium
Leaching rate is high, selenium, cadmium segregation ratio more thoroughly, of low cost, safety and environmental protection.
Raw material is cadmium selenide waste material in following embodiment, and wherein selenium mass fraction is 41.3%, and the mass fraction of cadmium is
58.7%。
Embodiment 1.
1）The CdSe powder that 396g is sieved with 100 mesh sieve is added into 3L autoclaves, by liquid-solid ratio 6:1 is added 2376ml
The liquid caustic soda solution of a concentration of 80g/L, closed reactor open stirring, control 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, reacts and is passed through circulating water after 4h to room temperature, by feed liquid in kettle into
Row filtering obtains one section of oxygen pressure alkali leaching leached mud and one section of oxygen pressure alkali leaching leachate.
The quality of wherein one section oxygen pressure alkali leaching leached mud（Dry weight）For 353.6g, detecting wherein Se contents through ICP-MS is
25.3%, Cd content are 65.7%.
2）It presses alkali leaching leached mud to be added in the autoclave of 3L one section of oxygen, is 4 by liquid-solid ratio:1 addition is a concentration of
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 and follows after reaction 2h
Ring is water-cooled to 60 DEG C, and filtering, obtained two sections of oxygen pressure alkali leaching leachate is back in one section of oxygen pressure alkali leaching leaching agent, two sections of oxygen
Press alkali leaching leached mud after washing is dried, quality 306.0g is 2.2%, Cd mass through ICP-MS detections wherein Se mass contents
Content is 75.7%.
In the present embodiment, it is 0.34% that total leaching rate of two sections of oxygen pressure alkali leaching Se, which is the total leaching rates of 95.8%, Cd,.
Embodiment 2.
1）The CdSe powder after 396g is sieved with 100 mesh sieve is added into 3L autoclaves, by liquid-solid ratio 5:1, it is added
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 reacting 4h
To 40 DEG C, feed liquid in kettle is filtered, obtains one section of oxygen pressure alkali leaching leached mud and one section of oxygen pressure alkali leaching leachate.
The quality of wherein one section oxygen pressure alkali leaching leached mud（Dry weight）For 350.4g, detecting wherein Se contents through ICP-MS is
23.9%, Cd content are 66.3%.
2）It presses alkali leaching leached mud to be added in the autoclave of 3L one section of oxygen, is 6 by liquid-solid ratio:1, it is added a concentration of
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 and follows after reaction 2h
Ring is water-cooled to 50 DEG C, and filtering, obtained two sections of oxygen pressure alkali leaching leachate is back in one section of oxygen pressure alkali leaching leaching agent, two sections of oxygen
Press alkali leaching leached mud after washing is dried, quality 305.6g is 1.9%, Cd mass through ICP-MS detections wherein Se mass contents
Content is 75.9%.
In the present embodiment, it is 0.26% that total leaching rate of two sections of oxygen pressure alkali leaching Se, which is the total leaching rates of 96.4%, Cd,.
Further include SeO in one section of oxygen pressure alkali leaching leaching agent in the present embodiment3 2-And SeO4 2-Ion.
Embodiment 3.
1）The CdSe powder after 396g is sieved with 100 mesh sieve is added into 3L autoclaves, by liquid-solid ratio 4:1, it is added
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 reacting 4h
To 40 DEG C, feed liquid in kettle is filtered, obtains one section of oxygen pressure alkali leaching leached mud and one section of oxygen pressure alkali leaching leachate.
The quality of wherein one section oxygen pressure alkali leaching leached mud（Dry weight）For 355.2g, detecting wherein Se contents through ICP-MS is
26.0%, Cd content are 65.4%.
2）It presses alkali leaching leached mud to be added in the autoclave of 3L one section of oxygen, is 5 by liquid-solid ratio:1, it is added a concentration of
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 and follows after reaction 2h
Ring is water-cooled to 50 DEG C, and filtering, obtained two sections of oxygen pressure alkali leaching leachate is back in one section of oxygen pressure alkali leaching leaching agent, two sections of oxygen
Press alkali leaching leached mud after washing is dried, quality 305.0g is 1.7%, Cd mass through ICP-MS detections wherein Se mass contents
Content is 75.9%.
In the present embodiment, it is 0.35% that total leaching rate of two sections of oxygen pressure alkali leaching Se, which is the total leaching rates of 96.8%, Cd,.
Further include SeO in one section of oxygen pressure alkali leaching leaching agent in the present embodiment3 2-And SeO4 2-Ion.
In above example, obtained one section of oxygen pressure alkali leaching leachate can be directly used for evaporating, concentrating and crystallizing, and recycling obtains
Sodium selenite crystal, obtained two sections of oxygen pressure alkali leaching leached mud is cadmium hydroxide crystal, can be used for recycling cadmium.
The present invention presses alkali leaching 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 alkali leaching is pressed, avoids the selenium excessive oxidation in cadmium selenide at sodium selenate, selenium is only made to enter in the form of sodium selenite
Solution；Furthermore two sections of oxygen pressure alkali leachings use higher partial pressure of oxygen and the higher leaching agent of naoh concentration, to ensure one section of oxygen
Selenium in pressure alkali leaching leached mud leaches completely.Method provided by the invention, by leaching selenium, the leaching of selenium from cadmium selenide waste material
Rate is high, and selenium and cadmium separative efficiency are high, of low cost, safety and environmental protection.
Although being example purpose, the preferred embodiment of the present invention, the ordinary skill people of this field are had been disclosed for
Member will realize in the case where not departing from the scope and spirit of the present invention disclosed in appended claims, various to change
Into, increase and substitution be possible.
Claims (7)
1. a kind of method for leaching selenium in waste material from cadmium selenide, which is characterized in that alkali leaching is pressed using two sections of oxygen, including：
Cadmium selenide waste material is first subjected to one section of oxygen pressure alkali leaching, original of the leached mud that one section of oxygen pressure alkali soaks as two sections of oxygen pressure alkali leachings
The leachate of material, two sections of oxygen pressure alkali leachings is back in the leaching agent of one section of oxygen pressure alkali leaching；
One section of oxygen pressure alkali leaching and two sections of oxygen press alkali leaching to be carried out in autoclave, and are passed through oxygen as oxidation
Agent；
Partial pressure of oxygen is 0.3~0.5MPa in autoclave when one section of oxygen pressure alkali leaching；High pressure when two sections of oxygen pressure alkali leaching
Partial pressure of oxygen is 0.8~1.2MPa in reaction kettle；
Naoh concentration is 80~120g/L in the leaching agent of one section of oxygen pressure alkali leaching；The leaching of two sections of oxygen pressure alkali leaching
Agent is the sodium hydroxide solution of 120~160g/L.
2. the method for leaching selenium in the waste material according to claim 1 from cadmium selenide, which is characterized in that one section of oxygen presses alkali
The leaching agent of leaching further includes SeO3 2-And/or SeO4 2-Ion.
3. the method for leaching selenium in the waste material according to claim 1 from cadmium selenide, which is characterized 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).
4. the method for leaching selenium in the waste material according to claim 1 from cadmium selenide, which is characterized in that two sections of oxygen presses alkali
The extraction temperature of leaching is 120~180 DEG C.
5. the method for leaching selenium in the waste material according to claim 1 from cadmium selenide, which is characterized in that two sections of oxygen presses alkali
Soak equal 2~4h of leaching.
6. the method for leaching selenium in the waste material according to claim 1 from cadmium selenide, which is characterized in that two sections of oxygen presses alkali
After leaching, it is passed through circulating water, reactor temperature is made to be less than 60 DEG C.
7. according to the method for leaching selenium in any slave cadmium selenide waste material of claim 1~6, which is characterized in that the selenium
It is 41.3% that Cd mass fractions, which are 58.7%, Se mass content scores, in cadmium waste material；The cadmium selenide waste material need to be crushed
The granularity of sieving, control cadmium selenide waste material is not more than 0.15mm.
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| WO1989012700A1 (en) * | 1988-06-17 | 1989-12-28 | Fmc Technologies Limited | Recovery of high purity selenium from ores, scrubber sludges, anode slime deposits and scrap |
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