CN102352435A - Efficient leaching technology of metal ions in chrysotile nanofiber - Google Patents
Efficient leaching technology of metal ions in chrysotile nanofiber Download PDFInfo
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- CN102352435A CN102352435A CN2011103313127A CN201110331312A CN102352435A CN 102352435 A CN102352435 A CN 102352435A CN 2011103313127 A CN2011103313127 A CN 2011103313127A CN 201110331312 A CN201110331312 A CN 201110331312A CN 102352435 A CN102352435 A CN 102352435A
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Abstract
The invention provides an efficient leaching technology of metal ions in chrysotile nanofiber and particularly relates to an efficient leaching technology of metal ions in silicon oxide nanofiber prepared from chrysotile, belonging to the fields of mineral materials and mineral processing. The efficient leaching technology uses chrysotile nanofiber as a raw material and one or more of low concentration sulphuric acid, hydrochloric acid and nitric acid as a leaching agent; and the countercurrent leaching technology with 2-4 sections is adopted, the efficient leaching of chrysotile nanofiber is performed for a proper time at the atmospheric pressure and at a proper temperature, the acid-leaching product is washed with dilute acid and water in sequence, and finally the silicon oxide nanofiber with higher purity can be obtained. By adopting the technology, the efficient leaching of metal ions can be effectively realized while the large length-diameter ratio of the product silicon oxide nanofiber can be maintained; and the equipment is simple, the operations are convenient, the acid consumption is extremely low, the pH value of the discharged tail acid is about 1 after the balance of the system, the subsequent magnesium extraction and neutralization treatment are performed easily and the environmental cost is reduced extremely.
Description
Technical field
The present invention relates to the high-efficiency leaching process of metal ion in a kind of chrysotile nano fiber, particularly utilize the method for the efficient leaching of metal ion in the monox nanometer fiber of chrysotile preparation, belong to mineral material and mineral manufacture field.
Background technology
Serpentine is a kind of natural magnesium silicate minerals that contains; Be 1: 1 type layer silicate mineral, mainly be divided into lizardite, antigorite and three mineral species of chrysotile by the difference of internal crystal structure by tetrahedral si-o film and brucite octahedral sheet be combined into.The desirable chemical formula of serpentine is Mg
3[Si
2O
5] (OH)
4, wherein MgO content is 43.0%, SiO
2Content is 44.1%.In addition, a lot of metals are present among the serpentine lattice with the substituted mode of isomorph, comprise rare metals such as nickel, titanium, chromium, palladium.As far back as eighties of last century forties, just there is United States Patent (USP) to report the extraction and application of magnesium in the serpentine.In decades subsequently, lot of domestic and international investigator has proposed about the method for comprehensive utilization of serpentine and the development technique of magnesium silicon series product.Realizing the prerequisite of these methods and technology, is efficiently the magnesium in the serpentine, element silicon to be separated through metallurgical method (comprising pyrogenic process and wet method).Wherein, wet method acid immersion has been proved to be a kind of treatment technology effectively, can realize the leaching of magnesium to a great extent.The magnesium liquid that leaching obtains can be used for preparing magnesium products, and the filter cake that obtains then can be used to prepare the silicon product, like organosilicon, white carbon black, molecular sieve etc.
About the acidleach of serpentine minerals, existing numerous papers and patent report.Comparative maturity and traditional technology are to adopt the mineral acid of high density under the situation of heating, serpentine to be carried out the normal pressure leaching at present; Can more fully remove metal ion wherein, carry out the work that follow-up white residue utilization and leach liquor extract metals such as magnesium then.Domestic a lot of researchist adopts similar technology serpentine and mine tailing resource thereof to be carried out the comprehensive utilization of magnesium, silicon.This type technical process is simple; Can effectively utilize resources such as magnesium in the serpentine, silicon; But weak point is that the concentration of used acid is too high; Concentrated hydrochloric acid as 31% (patent 200610030750.9 etc.), vitriol oil (patent 200810058252.4,01131802.3 etc.) of 40～60% etc.; This has not only increased the burden of equipment and personnel in the leaching process; And the tail that forms acid pH value is low excessively, is unfavorable for neutralizing treatment, or environment is caused potential hazard.
Except above-mentioned direct leaching process, the report of new extract technology has appearred in recent years.For example, people such as Wan Yong (Wan Yong etc., mineral journal, 2004,24 (4): 347-350) utilize microwave exposure to carry out the sulfuric acid leaching research of serpentine, can improve the leaching efficiency of serpentine effectively, but preferable sulfuric acid concentration is still very high, is about 50%.People such as Wang Hui (patent 200710035025.5) have reported that a kind of circulated in countercurrent technology leaches the metal in the serpentine, can reduce the leaching cost effectively, help reducing follow-up purifying treatment process cost, and comprehensive high-efficiency ground reclaims metals resources wherein.But can find out that from embodiment employed acid concentration is still higher, be about 40% like sulfuric acid.
We have obtained the patent of invention (patent name: the preparation method of chrysotile nano fiber of chrysotile nano fiber preparation in earlier stage; The patent No.: ZL200610031635.3), the chrysotile nano fiber diameter that obtains is at tens nanometer, and length is ten several microns, surface coverage layer of surface promoting agent adsorption layer.Fall the metal ion in the chrysotile nano fiber through the acidleach corrosion, can low cost, high-level efficiency, prepare the monox nanometer fiber on a large scale, have wide application prospect in various fields.Different with the employed serpentine of common leaching (containing chrysotile) is that therefore this chrysotile nano fiber has very strong reactive behavior and thickening property owing to have minimum size and great specific surface area.Though the metal in this chrysotile nano fiber can be effectively leached in the acid of high density, form high-purity mangesium oxide silicon, in leaching process, cause the fracture of fiber easily, reduce the length-to-diameter ratio of product monox nanometer fiber.Because the thickening property of this chrysotile nano fiber is very strong, lower liquid-solid ratio makes agitation leach to carry out simultaneously.Because characteristics such as the not anti-strong acid of this kind chrysotile nano fiber, thickening property, what forefathers had developed is that the serpentine acid leaching technology of characteristic can't be applied to wherein with high concentrated acid, low liquid-solid ratio.Therefore; These characteristics to chrysotile nano fiber; Exploitation is the chrysotile nano fiber high-efficiency leaching process of characteristics with low acid concentration, big liquid-solid ratio, adverse current; Could when effectively realizing the efficient leaching of metal ion, keep the big L/D ratio shape characteristic of product monox nanometer fiber.This has crucial meaning for the industrial application that chrysotile prepares the monox nanometer fiber.
Summary of the invention
The purpose of this invention is to provide that a kind of acid consumption is lower, equipment and operating process are simple, be fit to scale operation; And when can realize effectively that metal ion is efficient and leach, keep the efficient method that leaches of metal ion in the chrysotile nano fiber of big L/D ratio shape characteristic of product monox nanometer fiber.
Principle of the present invention is: because dispersion treatment technology, the chrysotile nano fiber surface is coated with layer of surface promoting agent rete, makes chrysotile nano fiber have certain solidity to corrosion to diluted acid.Under the effect of acid; The rete and the crystalline structure on chrysotile nano fiber surface are destroyed; Metal ion in the lattice changes liquid phase over to by solid phase in leaching process; When realizing that metal ion constantly leaches; Also constantly reduce leaching velocity; Until reaching chemical equilibrium, can only realize the leaching of most metal ions.Owing to be that adverse current leaches, thus to the acid that solid-liquid separation obtains after the back one section leaching be used for the leaching of the last period and handle, so be equivalent to adopt eo-acid to leach processing once more, can realize the leaching fully of metal ion basically.Because the zero point that leaches product monox nanometer fiber is about 2, and specific surface area is huge, so the metal ion in the leach liquor very easily is adsorbed in its surface, therefore need carry out repetitive scrubbing to remove the metal ion of this part physical adsorption and electrostatic adhesion.And contain little metal ions such as Fe, Al, Mn in the chrysotile inevitably; Rising along with washing process pH value; Can form hydroxide colloid and be deposited on the monox nanometer fiber, thus at first must adopt the acid solution washing, to remove these metal ions substantially.
In order to realize the object of the invention, also need consider following factor simultaneously: suitable acid concentration can guarantee that the high leaching yield of metal ionic reduces the acid consumption of whole leaching process simultaneously, can't cause the fracture of the monox nanometer fiber of formation in (1) leach liquor; (2) suitable leaching system solids concn not only makes leaching process efficiently to carry out, and reduces the acid consumption of leaching process simultaneously; (3) Shi Yi stirring velocity can ensure effectively carrying out of mass transfer process; (4) the certain reaction temperature is guaranteed higher metal ion leaching yield; (5) reasonably the reaction times makes that leaching reaction can fully carry out; (6) suitable wash conditions can guarantee that metal ion effectively comes off from the leached mud surface, helps the formation of high-purity mangesium oxide silicon nanofiber.
We pass through repeated tests; Explored and leached material chrysotile nano fiber and the mass volume ratio of leach liquor, the correlation parameters such as rotating speed of leaching reaction times, temperature and agitator in sour kind and concentration in the suitable leach liquor, the leaching system; When guaranteeing the efficient leaching of metal ion; Significantly reduce sour consumption, and guaranteed the length-to-diameter ratio of product monox nanometer fiber.
For achieving the above object, the technical scheme that the present invention adopts is following:
The high-efficiency leaching process of metal ion in a kind of chrysotile nano fiber; Chrysotile nano fiber joined carry out adverse current in the lower concentration acid that the hydrogen ion volumetric molar concentration is 0.25～1mol/L and leach, described adverse current extracting stage comprises two sections, three sections or four sections adverse current leaching process; Chrysotile nano fiber adds before first section leaching, and following current to final stage leaches the back and discharges; Diluted acid in the end adds before one section leaching, discharges after adverse current to the first section leaching; Said leaching is carried out under normal pressure, and the solid-to-liquid ratio that each section leaches system is 1: 20～1: 80g/ml, each section extraction temperature are 50～100 ℃, and each section extraction time is 0.5～4h; After leaching, the gained leached mud is earlier after after diluted acid and the water washing, can get the higher monox nanometer fiber of purity; Follow-up magnesium or the neutralizing treatment put forward carried out in the tail acid of discharging.
Described leaching agent diluted acid is selected from one or more in sulfuric acid, hydrochloric acid, the nitric acid.
Described diluted acid is preferably dilute sulphuric acid, and the hydrogen ion volumetric molar concentration of diluted acid is preferably 0.5～1mol/L.
Described adverse current extract technology is preferably three sections.
During said leaching, preferred solid-to-liquid ratio is 1: 30～1: 60g/ml, extraction temperature are 80～100 ℃, and the reaction times is 1.5～3 hours, stir during leaching, and stirring velocity is 400～700 rev/mins.
The leaching auxiliary agent that can add chrysotile nano fiber mass ratio 0.1～10% during leaching leaches acid or salt that auxiliary agent comprises fluorochemical class, lemon acids, oxalic acid class.
It is 0.5～3% that said leaching auxiliary agent preferably adds mass ratio.
The washing process of said leached mud comprises that successively 1～2 section pH value is 1～2 diluted acid (sulfuric acid, hydrochloric acid or nitric acid all can) agitator treating 10-120 minute and 2～6 sections water washings, and wash temperature is room temperature～100 ℃.
After washing was accomplished, the pH value of may command final product monox nanometer fiber was 4～7.
Said adverse current leaching process can guarantee that metal ion is leached by efficient in the chrysotile nano fiber; The weak acid scrubbing process can guarantee to stick to through electrostatic adhesion or physisorption the effective elimination of the metal ion that leaches product monox nanometer fiber surface, avoids forming metal hydroxides colloidal precipitation simultaneously at the monox nanometer fiber surface; The water washing process can be adjusted in slightly acidic-neutral range the pH value of product monox nanometer fiber.So, can form the monox nanometer fiber that purity is higher, the pH value is moderate.Hydrogen ion concentration is lower in the produced simultaneously tail acid, and what be easy to the later stage puies forward magnesium and neutralizing treatment.
The pH value of the tail acid of discharging after said first section leaching is 0.5～1.5.
Said acid cleaning process, preferred two sections pickling, washing is preferably about 2 with the pH value of acid, and wash temperature is preferably 80～100 ℃, and the agitator treating time is preferably 30～60 minutes.
Said washing process, preferred four sections washing process.
Compare with existing serpentine minerals leaching-out technique, the present invention has following advantage:
(1) the present invention is under normal pressure; With in sulfuric acid, hydrochloric acid, the nitric acid one or more as leaching agent; Leach and the acid elution mode realizes the efficient leaching of metal ion in the chrysotile nano fiber, the monox nanometer fiber of preparation higher degree from chrysotile nano fiber effectively with adverse current.
(2) acid solutions used in the present invention is very low, and hydrogen ion concentration is no more than 1mol/L, is difficult for causing the fracture of acidleach product monox nanometer fiber, can make the monox nanometer fiber of big L/D ratio.
(3) employed acid amount used in the present invention is very little, and after leaching, the sour pH value of the tail of discharging is easy to carry out follow-up magnesium and the neutralizing treatment put forward about 1, greatly reduced Environmental costs.
Description of drawings
Fig. 1: two sections adverse current leaching-out technique synoptic diagram;
Fig. 2: three sections adverse current leaching-out technique synoptic diagram;
Fig. 3: four sections adverse current leaching-out technique synoptic diagram.
Embodiment
The present invention is further specified by the following example, but is not subjected to the restriction of these embodiment.
Chrysotile nano fiber in the embodiment of the invention is according to the preparation of the method for patent ZL200610031635.3.
Embodiment 1
Two sections hydrochloric acid adverse currents leach, and flow process is seen Fig. 1.Adopt hydrogen ion concentration be the hydrochloric acid soln of 0.8mol/L as leaching agent, by 1: the solid-to-liquid ratio of 50g/ml adds hydrochloric acid, and each section extraction time is 2h, and temperature is 80 ℃, 500 rev/mins of stirring velocitys.Add fresh chrysotile nano fiber solid at first section, add fresh acid at second section.The solid trend is one section → two sections, and the trend of liquid is two sections → one section.While is at the leaching auxiliary agent oxalic acid of second section adding 2%.PH is carried out in the tail acid of discharging after first section leaching at every turn and measure, after 8～10 batches of leachings, the pH value stabilization of tail acid is about 0.8, and adverse current leaching system reaches balance.The solid of second section discharge obtains purity greater than 93% monox nanometer fiber after the hydrochloric acid of pH=2 and deionized water repeatedly wash.
Embodiment 2
Operating process is with embodiment 1, just adopt hydrogen ion concentration be the hydrochloric acid soln of 0.5mol/L as leaching agent, by 1: the solid-to-liquid ratio of 80g/ml adds hydrochloric acid, and each section extraction time is 4h, and temperature is 95 ℃, 700 rev/mins of stirring velocitys.Leaching auxiliary agent Trisodium Citrate second section adding 8%.PH is carried out in the tail acid of discharging after first section leaching at every turn and measure, after 8～10 batches of leachings, the pH value stabilization of tail acid is about 0.8, and adverse current leaching system reaches balance.The solid of second section discharge obtains purity greater than 92% monox nanometer fiber after the hydrochloric acid of pH=2 and deionized water repeatedly wash.
Embodiment 3
Operating process is with embodiment 1, just adopt hydrogen ion concentration be the hydrochloric acid soln of 1.0mol/L as leaching agent, by 1: the solid-to-liquid ratio of 40g/ml adds hydrochloric acid, and each section extraction time is 1h, and temperature is 60 ℃, 400 rev/mins of stirring velocitys.Leaching auxiliary agent sodium oxalate second section adding 5%.PH is carried out in the tail acid of discharging after first section leaching at every turn and measure, after 8～10 batches of leachings, the pH value stabilization of tail acid is about 0.8, and adverse current leaching system reaches balance.The solid of second section discharge obtains purity greater than 92% monox nanometer fiber after the hydrochloric acid of pH=2 and deionized water repeatedly wash.
Embodiment 4
Three sections sulfuric acid adverse currents leach, and flow process is seen Fig. 2.Adopt hydrogen ion concentration be the sulphuric acid soln of 0.5mol/L as leaching agent, by 1: the solid-to-liquid ratio of 50g/ml adds sulfuric acid, and each section extraction time is 2h, and temperature is 90 ℃, 500 rev/mins of stirring velocitys.。Add fresh chrysotile nano fiber solid at first section, add fresh acid at the 3rd section.The solid trend is one section → two sections → three sections, and the trend of liquid is three sections → two sections → one section.While is at the leaching auxiliary agent oxalic acid of the 3rd section adding 1%.PH is carried out in the tail acid of discharging after first section leaching at every turn and measure, after 8～10 batches of leachings, the pH value stabilization of tail acid is about 1.2, and adverse current leaching system reaches balance.The solid of the 3rd section discharge obtains purity greater than 96% monox nanometer fiber after the sulfuric acid of pH=2 and deionized water repeatedly wash.
Embodiment 5
Operating process is with embodiment 4, just adopt hydrogen ion concentration be the sulphuric acid soln of 0.4mol/L as leaching agent, by 1: the solid-to-liquid ratio of 60g/ml adds sulfuric acid, and each section extraction time is 4h, and temperature is 80 ℃, 600 rev/mins of stirring velocitys.Leaching auxiliary agent Hydrocerol A the 3rd section adding 8%.PH is carried out in the tail acid of discharging after first section leaching at every turn and measure, after 8～10 batches of leachings, the pH value stabilization of tail acid is about 1.2, and adverse current leaching system reaches balance.The solid of the 3rd section discharge obtains purity greater than 95% monox nanometer fiber after the sulfuric acid of pH=2 and deionized water repeatedly wash.
Embodiment 6
Operating process is with embodiment 4, just adopt hydrogen ion concentration be the sulphuric acid soln of 0.8mol/L as leaching agent, by 1: the solid-to-liquid ratio of 40g/ml adds sulfuric acid, and each section extraction time is 1.5h, and temperature is 70 ℃, 400 rev/mins of stirring velocitys.Leaching auxiliary agent oxalic acid the 3rd section adding 5%.PH is carried out in the tail acid of discharging after first section leaching at every turn and measure, after 8～10 batches of leachings, the pH value stabilization of tail acid is about 1.2, and adverse current leaching system reaches balance.The solid of the 3rd section discharge obtains purity greater than 95% monox nanometer fiber after the sulfuric acid of pH=2 and deionized water repeatedly wash.
Embodiment 7
Four sections sulfuric acid adverse currents leach, and flow process is seen Fig. 3.Adopt hydrogen ion concentration be the sulphuric acid soln of 0.8mol/L as leaching agent, by 1: the solid-to-liquid ratio of 50g/ml adds sulfuric acid, and each section extraction time is 2h, and temperature is 90 ℃, 400 rev/mins of stirring velocitys.Add fresh chrysotile nano fiber solid at first section, add fresh acid at the 4th section.The solid trend is one section → two sections → three sections → four sections, and the trend of liquid is four sections → three sections → two sections → one section.While is at the leaching auxiliary agent oxalic acid of the 4th section adding 1%.PH is carried out in the tail acid of discharging after first section leaching at every turn and measure, after 8～10 batches of leachings, the pH value stabilization of tail acid is about 1, and adverse current leaching system reaches balance.The solid of the 4th section discharge obtains purity and is about 99% monox nanometer fiber after the sulfuric acid of pH=2 and deionized water repeatedly wash.
Embodiment 8
Operating process is with embodiment 7, just adopt hydrogen ion concentration be the sulphuric acid soln of 0.5mol/L as leaching agent, by 1: the solid-to-liquid ratio of 80g/ml adds sulfuric acid, and each section extraction time is 4h, and temperature is 90 ℃, 600 rev/mins of stirring velocitys.Leaching auxiliary agent Trisodium Citrate the 4th section adding 8%.PH is carried out in the tail acid of discharging after first section leaching at every turn and measure, after 8～10 batches of leachings, the pH value stabilization of tail acid is about 1, and adverse current leaching system reaches balance.The solid of the 4th section discharge obtains purity and is about 98% monox nanometer fiber after the sulfuric acid of pH=2 and deionized water repeatedly wash.
Embodiment 9
Operating process is with embodiment 7, just adopt hydrogen ion concentration be the sulphuric acid soln of 1.0mol/L as leaching agent, by 1: the solid-to-liquid ratio of 40g/ml adds sulfuric acid, and each section extraction time is 1h, and temperature is 60 ℃, 400 rev/mins of stirring velocitys.Leaching auxiliary agent oxalic acid the 4th section adding 2%.PH is carried out in the tail acid of discharging after first section leaching at every turn and measure, after 8～10 batches of leachings, the pH value stabilization of tail acid is about 1, and adverse current leaching system reaches balance.The solid of the 4th section discharge obtains purity and is about 98% monox nanometer fiber after the sulfuric acid of pH=2 and deionized water repeatedly wash.
Claims (8)
1. the high-efficiency leaching process of metal ion in the chrysotile nano fiber; It is characterized in that; Chrysotile nano fiber joined carry out adverse current in the lower concentration acid that the hydrogen ion volumetric molar concentration is 0.25～1mol/L and leach, the described adverse current section of soaking comprises two sections, three sections or four sections adverse current leaching process; Chrysotile nano fiber adds before first section leaching, and following current to final stage leaches the back and discharges; Diluted acid in the end adds before one section leaching, discharges after adverse current to the first section leaching; Said leaching is carried out under normal pressure, and the solid-to-liquid ratio that each section leaches system is 1: 20～1: 80g/ml, each section extraction temperature are 50～100 ℃, and each section extraction time is 0.5～4h; After leaching, the gained leached mud is earlier after after diluted acid and the water washing, can get the higher monox nanometer fiber of purity; Follow-up magnesium or the neutralizing treatment put forward carried out in the tail acid of discharging.
2. the high-efficiency leaching process of metal ion is characterized in that in the chrysotile nano fiber according to claim 1, and described leaching agent diluted acid is selected from one or more in sulfuric acid, hydrochloric acid, the nitric acid.
3. the high-efficiency leaching process of metal ion is characterized in that in the chrysotile nano fiber according to claim 1 and 2, and described diluted acid is a dilute sulphuric acid, and the hydrogen ion volumetric molar concentration of diluted acid is 0.5～1mol/L.
4. the high-efficiency leaching process of metal ion is characterized in that in the chrysotile nano fiber according to claim 1, and described adverse current extract technology is three sections.
5. according to the high-efficiency leaching process of metal ion in claim 1 or the 4 described chrysotile nano fibers; It is characterized in that; During said leaching; Solid-to-liquid ratio is 1: 30～1: 60g/ml; Extraction temperature is 80～100 ℃; Reaction times is 1.5～3 hours, stirs during leaching, and stirring velocity is 400～700 rev/mins.
6. the high-efficiency leaching process of metal ion in the chrysotile nano fiber according to claim 1; It is characterized in that; Add the leaching auxiliary agent of chrysotile nano fiber mass ratio 0.1～10% during leaching, leach acid or salt that auxiliary agent comprises fluorochemical class, lemon acids, oxalic acid class.
7. the high-efficiency leaching process of metal ion is characterized in that in the chrysotile nano fiber according to claim 6, and it is 0.5～3% that said leaching auxiliary agent adds mass ratio.
8. the high-efficiency leaching process of metal ion in the chrysotile nano fiber according to claim 1; It is characterized in that; The washing process of said leached mud comprises that successively 1～2 section pH value is diluted acid agitator treating 10-120 minute and 2～6 sections water washings of 1～2, and wash temperature is room temperature～100 ℃.
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| CN103337597A (en) * | 2013-07-03 | 2013-10-02 | 中南大学 | Silicon oxide nanofiber and polymer composite transparent film, and preparation method and application of transparent film |
| CN103482628A (en) * | 2013-10-11 | 2014-01-01 | 西南科技大学 | Fibrous nanosilicon preparation method |
| CN104009224A (en) * | 2014-05-13 | 2014-08-27 | 昆明理工大学 | Method for synthesizing lithium iron silicate positive electrode material by using chrysotile asbestos as raw material |
| CN104009211A (en) * | 2014-05-13 | 2014-08-27 | 昆明理工大学 | Preparation method for porous silicon nanofiber/carbon composite material |
| CN105695738A (en) * | 2016-03-25 | 2016-06-22 | 武汉科技大学 | Deironing method for vanadium-bearing stone coal lixivium |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103337597A (en) * | 2013-07-03 | 2013-10-02 | 中南大学 | Silicon oxide nanofiber and polymer composite transparent film, and preparation method and application of transparent film |
| CN103337597B (en) * | 2013-07-03 | 2016-03-02 | 中南大学 | Silicon oxide nanofiber and polymer composite transparent film and its preparation method and application |
| CN103482628A (en) * | 2013-10-11 | 2014-01-01 | 西南科技大学 | Fibrous nanosilicon preparation method |
| CN103482628B (en) * | 2013-10-11 | 2016-01-20 | 西南科技大学 | The preparation method of fibrous nano silicon |
| CN104009224A (en) * | 2014-05-13 | 2014-08-27 | 昆明理工大学 | Method for synthesizing lithium iron silicate positive electrode material by using chrysotile asbestos as raw material |
| CN104009211A (en) * | 2014-05-13 | 2014-08-27 | 昆明理工大学 | Preparation method for porous silicon nanofiber/carbon composite material |
| CN105695738A (en) * | 2016-03-25 | 2016-06-22 | 武汉科技大学 | Deironing method for vanadium-bearing stone coal lixivium |
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Application publication date: 20120215 |