CN105460907B - A kind of extracting method of selenium-rich ore water soluble speciation - Google Patents
A kind of extracting method of selenium-rich ore water soluble speciation Download PDFInfo
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- CN105460907B CN105460907B CN201511003964.2A CN201511003964A CN105460907B CN 105460907 B CN105460907 B CN 105460907B CN 201511003964 A CN201511003964 A CN 201511003964A CN 105460907 B CN105460907 B CN 105460907B
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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
- C01B19/001—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
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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
- C01B19/02—Elemental selenium or tellurium
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Abstract
The present invention relates to a kind of extracting methods of selenium-rich ore water soluble speciation, include the following steps：S1：Selenium-rich ore (bone coal) is provided and is crushed, Rich selenium ore powders are obtained；S2：Sodium bicarbonate is provided, and Rich selenium ore powders and sodium bicarbonate are pressed to 5: 1 quality proportioning, is mixed with water and is tuned into paste, be squeezed into shot-like particle and dry；S3：Shot-like particle is placed in be sintered two hours in sintering furnace and obtains sintering feed；S4：Hot water stirs are added in sintering feed to extract 2 hours；S5：It is spare to centrifuge or filter to take the first supernatant, 0.1mol K are added in remaining residue2HPO4+KH2PO4Solution, stirring and leaching centrifuge after 2 hours, take the second supernatant spare, and all supernatants are mixed；S6：By all supernatants by vermiculite filter element filtering, selenium-rich aqueous solution is obtained.The extracting method of selenium-rich ore (bone coal) water soluble speciation is simple, efficient, environmental-friendly, at low cost, water soluble speciation recovery rate is high.
Description
Technical field
The present invention relates to a kind of extracting method of selenium more particularly to a kind of extracting methods of selenium-rich ore water soluble speciation.
Background technology
Dissipated metal selenium be widely used in metallurgical industry, electronics industry, national defense industry, xerography, glass, medicine and
The fields such as agricultural are constantly widened with the application field of selenium, and international market also increases the demand of selenium year by year.It is dilute due to selenium
Sexual, directly recycling is infeasible from ore, and the byproduct generated in heavy metal sulphide ore smelting process is recycling selenium
The smelting smoke dust that important sources, especially the anode mud of copper electroplating and processing sulphide ore generate is that the world today carries the main next of selenium
Source.
It is domestic at present mainly to use solvent extraction, ultravacuum volatility process, soda roasting method etc. by selenium and other impurity point
It leaves and.But these methods are compared with complex procedures, pollution is big, technological process is long, the recovery rate of selenium is relatively low.Therefore, from selenium-rich mine
It is current main research direction that a kind of method simple, efficient, environmental-friendly, at low cost, that recovery rate is high is developed in stone.
Invention content
The purpose of the present invention is being directed to above-mentioned present situation, it is high and at low cost to provide a kind of recovery rate of selenium-rich ore water soluble speciation
Selenium-rich ore (bone coal) water soluble speciation extracting method.
The technical solution adopted by the present invention：A kind of extracting method of selenium-rich ore water soluble speciation, includes the following steps：S1：
Selenium-rich ore (bone coal) is provided, and the selenium-rich ore is crushed in mineral smashing machine, obtains Rich selenium ore powders；S2：Carbon is provided
Sour hydrogen sodium, and the Rich selenium ore powders and the sodium bicarbonate are mixed with water by 5: 1 quality proportioning and are tuned into paste, it squeezes
It is pressed into shot-like particle and dries；S3：The shot-like particle is placed in sintering furnace, the sintering furnace is maintained at 450-600 DEG C, when sintering
Between be two hours, obtain sintering feed；S4：80-90 DEG C of hot water, stirring and leaching 2 hours are added in the sintering feed；S5：Centrifugation
Or to filter to take the first supernatant (or first filtered fluid) spare, and 0.1mol K are added in remaining residue2HPO4+KH2PO4Solution,
After stirring and leaching 2 hours, it is spare to centrifuge or filter to take the second supernatant (or second filtered fluid), and will be on spare described first
Clear liquid and the mixing of the second supernatant；S6：By all supernatants (or filtered fluid) by vermiculite filter element filtering, filtered fluid by sun from
Sub- exchange column obtains selenium-rich aqueous solution.
The present invention effect be：The extracting method of selenium-rich ore (bone coal) water soluble speciation is simple, it is efficient, environmental-friendly,
At low cost, water soluble speciation recovery rate is high.
Further, in step S5,0.1mol K are added2HPO4+KH2PO4After stand for 24 hours, when pH value be 7 when be stirred for
Extraction.
Further, in step S4, the solid-to-liquid ratio of the sintering feed and the water is 1: 25.
Further, in step S5,0.1mol K are added in remaining residue2HPO4+KH2PO4When solution, solid-to-liquid ratio
According to 1: 15 distribution.
Further, in step S1, the selenium-rich ore is crushed to 80 mesh.
Further, in step S2, a diameter of 1-2mm of the shot-like particle.
Further, in step S4, added water is 80-90 DEG C of hot water.
Further, in step S6, all supernatants be put into vermiculite impregnate 8 hours after filter, filtered fluid by sun from
Subtree Ester exchange obtains water soluble speciation solution.
Description of the drawings
Fig. 1, which show a kind of the step of extracting method of selenium-rich ore water soluble speciation provided by the invention, to scheme.
Specific implementation mode
The principle and features of the present invention will be described below with reference to the accompanying drawings, and the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the present invention.
Referring to Fig. 1, being a kind of extracting method of selenium-rich ore water soluble speciation provided by the invention, include the following steps：
S1：Selenium-rich ore (bone coal) is provided, and the selenium-rich ore is crushed in mineral smashing machine, obtains selenium-rich mine
Powder.In this present embodiment, the selenium content of the selenium-rich ore is 211mg/kg, and the selenium-rich ore is crushed to 80 mesh.
S2：Sodium bicarbonate is provided, and the Rich selenium ore powders and the sodium bicarbonate are mixed with water by 5: 1 proportionings
It is tuned into paste, be squeezed into shot-like particle and is dried.In this present embodiment, sodium bicarbonate 10g, Rich selenium ore powders 50g are provided, squeezed
A diameter of 1-2mm of the shot-like particle of formation.
S3：The shot-like particle is placed in sintering furnace, the sintering furnace is maintained at 450-600 DEG C, and sintering time is two small
When, obtain sintering feed.In this present embodiment, which is placed in Muffle furnace.
S4：80-90 DEG C of hot water, stirring and leaching 2 hours are added in the sintering feed.In this present embodiment, the sintering feed
Solid-to-liquid ratio with the hot water is 1: 25.In this present embodiment, hot water 1000ml is added.
S5：It is spare to centrifuge or filter to take the first supernatant (or first filtered fluid), 0.1mol is added in remaining residue
K2HPO4+KH2PO4Solution after standing 24 hours, after stirring and leaching when pH value is 72 hours, centrifuges or filters to take the second supernatant
Liquid (or second filtered fluid) is spare, and spare first supernatant and the second supernatant are mixed.In this present embodiment, it adopts
It is centrifugation, 500ml is added in remaining residue after obtaining the first supernatant 920ml in centrifugation time 20min
0.1mol K2HPO4+KH2PO4When solution, solid-to-liquid ratio is shaken 2 hours in reciprocating oscillator at room temperature according to 1: 15 distribution,
20min is centrifuged at room temperature, obtains the second supernatant 475ml.In this way, the first supernatant and the total 1395ml of the second supernatant.
S6：By all supernatants (or filtered fluid) by vermiculite filter element filtering, filtered fluid is obtained by cation exchange column
Selenium-rich aqueous solution.In this present embodiment, all supernatants be put into 50g vermiculites impregnate 8 hours after filter, filtered fluid by sun from
Subtree Ester exchange obtains water soluble speciation solution 1160ml, and the selenium content of the water soluble speciation solution is 5.8mg/l.
The selenium content of the selenium-rich ore is 211mg/kg, and provides Rich selenium ore powders 50g, and such raw material contains selenium
10.55mg；Water soluble speciation solution 1160ml, and the selenium content of the water soluble speciation solution is 5.8mg/l, contains selenium in such solution
6.73mg.In this way, the recovery rate according to aqueous solution selenium is 6.73/10.55=63.79%, recovery rate is higher；In addition, the selenium-rich
The extracting method of ore (bone coal) water soluble speciation is simple, efficient, environmental-friendly, at low cost.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of extracting method of selenium-rich ore water soluble speciation, it is characterised in that：Include the following steps：
S1：Selenium-rich ore is provided, and the selenium-rich ore is crushed in mineral smashing machine, obtains Rich selenium ore powders；
S2：Sodium bicarbonate is provided, and the Rich selenium ore powders and the sodium bicarbonate are pressed 5：1 quality proportioning adds water mixing equal
It is even at paste, be squeezed into shot-like particle and dry；
S3：The shot-like particle is placed in sintering furnace, the sintering furnace is maintained at 450-600 DEG C, and sintering time is two hours, is obtained
To sintering feed；
S4：It is added water in the sintering feed, the solid-to-liquid ratio of the sintering feed and the water is 1:25, added water is 80-90 DEG C
Hot water, stirring and leaching 2 hours；
S5：It is spare to centrifuge or filter to take the first supernatant, 0.1molK is added in remaining residue2HPO4+KH2PO4Solution, stirring
It after extraction 2 hours, centrifuges or filters to take that the second supernatant is spare, and spare first supernatant and the second supernatant are mixed
It closes；
S6：By all supernatants by vermiculite filter element filtering, filtered fluid obtains selenium-rich aqueous solution by cation exchange column.
2. the extracting method of selenium-rich ore water soluble speciation as described in claim 1, it is characterised in that：In step S5, it is added
0.1mol K2HPO4+KH2PO4After stand for 24 hours, when pH value be 7 when be stirred for extracting.
3. the extracting method of selenium-rich ore water soluble speciation as claimed in claim 2, it is characterised in that：In step S5, in residue
Residue in 0.1mol K are added2HPO4+KH2PO4When solution, solid-to-liquid ratio is according to 1:15 distribution.
4. the extracting method of selenium-rich ore water soluble speciation as described in claim 1, it is characterised in that：In step S1, the richness
Selenium ore is crushed to 80 mesh.
5. the extracting method of selenium-rich ore water soluble speciation as described in claim 1, it is characterised in that：In step S2, the grain
A diameter of 1-2mm of shape object.
6. the extracting method of selenium-rich ore water soluble speciation as described in claim 1, it is characterised in that：In step S6, this is all
Supernatant is put into after vermiculite impregnates 8 hours and filters, and filtered fluid obtains water soluble speciation solution by cation resin exchange.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106588177A (en) * | 2016-11-30 | 2017-04-26 | 广州市瑞硒康生物科技有限公司 | Culture method for selenium-rich lucid ganoderma |
| CN107333978A (en) * | 2016-11-30 | 2017-11-10 | 广州市瑞硒康生物科技有限公司 | A kind of animal Selenium-rich nutrient solution |
| CN107337500A (en) * | 2016-11-30 | 2017-11-10 | 广州市瑞硒康生物科技有限公司 | A kind of edible mushroom selenium-rich nutritive element |
| CN106576780A (en) * | 2016-11-30 | 2017-04-26 | 广州市瑞硒康生物科技有限公司 | Cultivating method for selenium-rich cardamine hupingshanesis and extracting method for selenium-rich cardamine hupingshanesis |
| CN107673315A (en) * | 2017-10-19 | 2018-02-09 | 河北工程大学 | A kind of method using the extraction selenium of bone coal containing selenium |
| CN109734503A (en) * | 2017-10-31 | 2019-05-10 | 湖南德禾农业电商科技有限公司 | A kind of selenium-rich tea oil uses fertilizer and preparation method thereof |
| CN109734494A (en) * | 2017-10-31 | 2019-05-10 | 湖南德禾农业电商科技有限公司 | A kind of dedicated selenium-rich fertilizer of peach and preparation method thereof |
| CN110333209A (en) * | 2019-07-11 | 2019-10-15 | 恩施土家族苗族自治州农业科学院(恩施土家族苗族自治州硒应用技术与产品开发研究院) | A kind of detection method of soil available Se |
| CN110367042A (en) * | 2019-08-28 | 2019-10-25 | 黑龙江坤健农业股份有限公司 | A kind of Se-rich lucid ganoderma bacterium bag breeding method |
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| CN102747225B (en) * | 2012-07-10 | 2013-08-07 | 中南大学 | Method for comprehensively recycling copper, selenium and uranium from stone coal extraction vanadic acid immersion liquid |
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