CN102249239A - Preparation method for preparing high-purity simple substance silicon from agricultural wastes - Google Patents
Preparation method for preparing high-purity simple substance silicon from agricultural wastes Download PDFInfo
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- CN102249239A CN102249239A CN 201110152177 CN201110152177A CN102249239A CN 102249239 A CN102249239 A CN 102249239A CN 201110152177 CN201110152177 CN 201110152177 CN 201110152177 A CN201110152177 A CN 201110152177A CN 102249239 A CN102249239 A CN 102249239A
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Abstract
The invention discloses a preparation method for preparing high-purity simple substance silicon from agricultural wastes, which comprises two simple steps: firstly, thermally decomposing the agricultural wastes into porous silicon dioxide powder, and then utilizing acid treatment and thermite reaction to remove the impurities from the porous silicon dioxide powder and reducing the porous silicon dioxide powder into the simple substance silicon. The agricultural wastes after being thermally decomposed have loose structures and the impurities therein can be easily removed, so that the purity of the acquired simple substance silicon is above 99% and a benefit is brought to the direct application or the further processing treatment. The preparation method for preparing high-purity simple substance silicon from agricultural wastes provided by the invention has the advantages that the cost of raw materials is low, the process flow is simple and the economic value and the application prospect are ultrahigh.
Description
Technical field
The present invention relates to the preparation method of compound, relate in particular to a kind of preparation method who prepares high purity elemental silicon from agricultural wastes.
Background technology
Agricultural wastes are meant the general name of the waste that produces in processes such as agriculture production, processing of farm products, mainly comprise shell fruit stone, stalk, rice husk, corn cob, branch fallen leaves and weeds etc., have enormous amount, renewable, the regeneration period short, characteristics such as biodegradable.Being rich in carbon and element silicon in these agricultural wastes, is important carbon silicon resource.China is a large agricultural country, and the annual number that produces is in hundred million tons various agricultural wastes, however most of agricultural wastes directly abandoned in the field, formed serious wasting of resources problem and environmental problem.The resource utilization of agricultural wastes and innoxious be the effective way that realizes agricultural sustainable development at present.
The application of elemental silicon and present Research: highly purified elemental silicon (Si) is the core material of information industry. contain a large amount of element silicons in the earth's crust, its content is only second to the oxygen of identical type.At present the preparation elemental silicon mainly adopts following method: 1. SiO
2Si+the 2Cl of+2C===Si+2CO ↑ 2.
2The SiCl of===
4SiCl
4+ 2H
2Si+the 4HCl of===.Two kinds of methods all need hot environment (more than 1200 degree).The application of elemental silicon is very extensive, is important semiconductor material by obtaining high-purity silicon single crystal after lifting.In silicon single crystal, mix the group III A element of trace, form p type silicon semiconductor; Mixing the VA family element of trace, form n type and p N-type semiconductorN and combine, will be excellent solar cell, be a kind of up-and-coming material aspect develop energy.With elemental silicon and ceramic mixed sintering, inherited the advantage separately of metal and pottery, remedied both birth defects again, be sintering metal, cosmonautic important materials.In addition, adopting elemental silicon is that raw material also can prepare high performance silica fiber, silicon sol and poly(oxygen-silicon) material etc.
Because agricultural wastes are through loosely organized after the pyrolysis, impurity is wherein easily removed, and prepares elemental silicon by agricultural wastes, and the purity of gained elemental silicon helps directly using or carrying out further processing treatment more than 99%.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of preparation method who prepares high purity elemental silicon from agricultural wastes is provided.
Preparation method's its step for preparing high purity elemental silicon from agricultural wastes is as follows:
1) 100 g agricultural wastes is fully pulverized, put into 400～1200
oCalcine 0.5～8 h in the C stove under air or oxygen atmosphere, obtaining main component is SiO
2Powder;
2) with gained SiO
2Powder soaks 1～24 h in the dilute hydrochloric acid solution of 0.1～1.0 mol/L, to remove impurity wherein; After the end with product 60～150
oStove is put in C oven dry back and 2～10 g metallic reducing agent powder thorough mixing, secluding air or under the protection of rare gas element 500～800
oC calcines 0.5～12 h; Take out the cooling back, and product soaks 1～24 h in the dilute hydrochloric acid solution of 0.1～1.0 mol/L, promptly gets purity after the oven dry and surpass 99% elemental silicon.
Described agricultural wastes are meant shell fruit stone, stalk, rice husk, corn cob, dry branches and fallen leaves or the weeds that form in agriculture production, processing of farm products process, its main component is siliceous organism; Described metallic reducing agent is one or both in simple substance magnesium powder or the aluminium powder; Described rare gas element is high pure nitrogen or high-purity argon gas.
What the present invention proposed prepares the method for high purity elemental silicon from agricultural wastes, and material cost is cheap, and technical process is simple; Because agricultural wastes are through loosely organized after the pyrolysis, impurity is wherein easily removed, so the purity of gained elemental silicon helps directly using or carrying out further processing treatment more than 99%; The method that the present invention proposes has extremely strong economic worth and application prospect.
Embodiment
Preparation method's its step for preparing high purity elemental silicon from agricultural wastes is as follows:
1) agricultural wastes are fully calcined under air or oxygen atmosphere.Because the main moiety of agricultural wastes is SiO
2And organism, in air or oxygen atmosphere, organism will be by abundant combustion decomposition, and the main component of gained powder is SiO
2
2) SiO
2The separation purification and the preparation of elemental silicon.The main component of the first step products therefrom is SiO
2Yet, wherein also contain K
2O, Fe
2O
3, Al
2O
3Deng impurity.Because SiO in agricultural wastes
2Be crosslinked distribution with organism, along with organic combustion decomposition, the structural system of agricultural wastes is with avalanche, and these oxide impurities are easy to be removed.Product is immersed in the oxide impurity that to remove in the dilute hydrochloric acid solution wherein.Remove behind the impurity with product oven dry back and a certain amount of metallic reducing agent powder such as thorough mixing such as metal magnesium powder, metallic aluminium powder secluding air or under the protection of rare gas element 500～800
oC calcines 0.5～12 h.Adopt the metallic reducing agent powder as reductive agent with add the synthesis temperature that thermal medium can significantly reduce elemental silicon (traditional method needs 1500
oMore than the C), not only reduced energy consumption, saved cost, also reduced demand to equipment.Concrete reaction equation following (is example with the magnesium powder):
SiO
2?+?2Mg?→?Si?+?2MgO
Si+2Mg → Mg
2Si(association reaction)
Impurity such as the magnesium oxide that generates, magnesium silicide can soak by dilute hydrochloric acid equally to be removed.Promptly get purity after the oven dry and surpass 99% elemental silicon.
Further specify the present invention below in conjunction with embodiment.
Embodiment 1: be raw material with the rice husk
1) 100 g rice husks is fully pulverized, put into 400
oCalcine 8 h in the C stove under air or oxygen atmosphere, obtaining main component is SiO
2Powder;
2) with gained SiO
2Powder soaks 24 h in the dilute hydrochloric acid solution of 0.1 mol/L, to remove impurity wherein; After the end with product 60
oStove is put in C oven dry back and 2 g metal magnesium powder thorough mixing, secluding air or under the protection of rare gas element 500
oC calcines 12 h; Take out the cooling back, soaks 24 h in the dilute hydrochloric acid solution of 0.1 mol/L, promptly gets purity and surpass 99% elemental silicon.
Embodiment 2: be raw material with the rice straw
1) 100 g rice straws is fully pulverized, put into 1200
oCalcine 0.5 h in the C stove under air or oxygen atmosphere, obtaining main component is SiO
2Powder;
2) with gained SiO
2Powder soaks 1 h in the dilute hydrochloric acid solution of 1.0 mol/L, to remove impurity wherein; After the end with product 150
oStove is put in C oven dry back and 10 g metallic aluminium powder thorough mixing, secluding air or under the protection of rare gas element 800
oC calcines 0.5 h; Take out the cooling back, soaks 1 h in the dilute hydrochloric acid solution of 1.0 mol/L, promptly gets purity and surpass 99% elemental silicon.
Embodiment 3: be raw material with wheat bran
1) 100 g wheat bran is fully pulverized, put into 500
oCalcine 6 h in the C stove under air or oxygen atmosphere, obtaining main component is SiO
2Powder;
2) with gained SiO
2Powder soaks 18 h in the dilute hydrochloric acid solution of 0.2 mol/L, to remove impurity wherein; After the end with product 70
oStove is put in C oven dry back and 4 g metal magnesium powder thorough mixing, secluding air or under the protection of rare gas element 600
oC calcines 8 h; Take out the cooling back, soaks 18 h in the dilute hydrochloric acid solution of 0.2 mol/L, promptly gets purity and surpass 99% elemental silicon.
Embodiment 4: be raw material with the maize straw
1) 100 g maize straws is fully pulverized, put into 600
oCalcine 4 h in the C stove under air or oxygen atmosphere, obtaining main component is SiO
2Powder;
2) with gained SiO
2Powder soaks 15 h in the dilute hydrochloric acid solution of 0.3 mol/L, to remove impurity wherein; After the end with product 90
oStove is put in C oven dry back and 6 g metallic aluminium powder thorough mixing, secluding air or under the protection of rare gas element 700
oC calcines 6 h; Take out the cooling back, soaks 15 h in the dilute hydrochloric acid solution of 0.3 mol/L, promptly gets purity and surpass 99% elemental silicon.
Embodiment 5: be raw material with the corn cob
1) 100 g corn cobs is fully pulverized, put into 700
oCalcine 3 h in the C stove under air or oxygen atmosphere, obtaining main component is SiO
2Powder;
2) with gained SiO
2Powder soaks 12 h in the dilute hydrochloric acid solution of 0.5 mol/L, to remove impurity wherein; After the end with product 100
oStove is put in C oven dry back and 8 g metal magnesium powder thorough mixing, secluding air or under the protection of rare gas element 650
oC calcines 9 h; Take out the cooling back, soaks 12 h in the dilute hydrochloric acid solution of 0.5 mol/L, promptly gets purity and surpass 99% elemental silicon.
Embodiment 6: be raw material with the straw
1) 100 g straws is fully pulverized, put into 1000
oCalcine 2 h in the C stove under air or oxygen atmosphere, obtaining main component is SiO
2Powder;
2) with gained SiO
2Powder soaks 5 h in the dilute hydrochloric acid solution of 0.8 mol/L, to remove impurity wherein; After the end with product 120
oStove is put in C oven dry back and 5 g metallic aluminium powder thorough mixing, secluding air or under the protection of rare gas element 750
oC calcines 3 h; Take out the cooling back, soaks 5 h in the dilute hydrochloric acid solution of 0.8 mol/L, promptly gets purity and surpass 99% elemental silicon.
Claims (4)
1. one kind prepares the preparation method of high purity elemental silicon from agricultural wastes, it is characterized in that its step is as follows:
1) 100 g agricultural wastes is fully pulverized, put into 400～1200
oCalcine 0.5～8 h in the C stove under air or oxygen atmosphere, obtaining main component is SiO
2Powder;
2) with SiO
2Powder soaks 1～24 h in the dilute hydrochloric acid solution of 0.1～1.0 mol/L, filter, and cleans 60～150
oStove is put in C oven dry back and 2～10 g metallic reducing agent powder thorough mixing, secluding air or under the protection of rare gas element 500～800
oC calcines 0.5～12 h; 1～24 h is soaked in cooling in the dilute hydrochloric acid solution of 0.1～1.0 mol/L, oven dry promptly gets purity and surpasses 99% elemental silicon.
2. a kind of preparation method who prepares high purity elemental silicon from agricultural wastes according to claim 1, it is characterized in that described agricultural wastes are meant shell fruit stone, stalk, rice husk, corn cob, dry branches and fallen leaves or the weeds that form in agriculture production, processing of farm products process, its main component is siliceous organism.
3. according to claim 1ly a kind ofly prepare the preparation method of high purity elemental silicon, it is characterized in that described metallic reducing agent is one or both in simple substance magnesium powder or the aluminium powder from agricultural wastes.
4. according to claim 1ly a kind ofly prepare the preparation method of high purity elemental silicon, it is characterized in that described rare gas element is high pure nitrogen or high-purity argon gas from agricultural wastes.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104030290A (en) * | 2014-06-30 | 2014-09-10 | 金之坚 | Method for producing nanometer silicon by adopting rice hull |
| CN104261411A (en) * | 2014-09-22 | 2015-01-07 | 江苏大学 | Preparation method of graphene-like magnesium silicide nanosheets |
| CN104556040A (en) * | 2014-12-03 | 2015-04-29 | 江苏大学 | Amorphous monatomic silicon ball as well as preparation method and application thereof |
| CN107934973A (en) * | 2017-11-24 | 2018-04-20 | 上海麟敏信息科技有限公司 | A kind of method and device that vegetalitas silicon is prepared by agricultural wastes |
| CN109585841A (en) * | 2018-12-05 | 2019-04-05 | 吉林大学 | A kind of lithium ion battery negative material and preparation method thereof, lithium ion cell electrode piece and lithium ion battery |
| CN109935807A (en) * | 2019-02-27 | 2019-06-25 | 福建翔丰华新能源材料有限公司 | A method of it aoxidizing sub- silicon and prepares lithium ion battery negative material |
| CN115156239A (en) * | 2022-07-15 | 2022-10-11 | 山东邦凯新材料有限公司 | Device and processing technology for preparing high-purity silicon dioxide by continuous recovery treatment of hazardous waste silica gel |
| WO2022225469A1 (en) * | 2021-04-19 | 2022-10-27 | Khon Kaen University | High-purity nanosilica and nanosilicon manufacturing process |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4214920A (en) * | 1979-03-23 | 1980-07-29 | Exxon Research & Engineering Co. | Method for producing solar cell-grade silicon from rice hulls |
-
2011
- 2011-06-08 CN CN 201110152177 patent/CN102249239A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4214920A (en) * | 1979-03-23 | 1980-07-29 | Exxon Research & Engineering Co. | Method for producing solar cell-grade silicon from rice hulls |
Non-Patent Citations (3)
| Title |
|---|
| 《Journal of Materials Science》 19851231 P Mishra et al. Production and purification of silicon by calcium reduction of rice-husk white ash 第4387-4391页，第1、2.1-2.4、4节 1-4 第20卷, * |
| 《Materials Science and Engineering》 19821231 H D Banerjee et al. Investigations on the production of silicon from rice husks by the magnesium method 第173-179页 1-4 第52卷, * |
| 《Solar Energy Materials》 19821231 D N Bose et al. Large grain polycrystalline silicon from rice husk 第319-321页，第2节 3 第7卷, * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104030290A (en) * | 2014-06-30 | 2014-09-10 | 金之坚 | Method for producing nanometer silicon by adopting rice hull |
| CN104030290B (en) * | 2014-06-30 | 2016-03-09 | 金之坚 | The method of nano-silicon is produced with rice husk |
| CN104261411A (en) * | 2014-09-22 | 2015-01-07 | 江苏大学 | Preparation method of graphene-like magnesium silicide nanosheets |
| CN104556040A (en) * | 2014-12-03 | 2015-04-29 | 江苏大学 | Amorphous monatomic silicon ball as well as preparation method and application thereof |
| CN107934973A (en) * | 2017-11-24 | 2018-04-20 | 上海麟敏信息科技有限公司 | A kind of method and device that vegetalitas silicon is prepared by agricultural wastes |
| CN109585841A (en) * | 2018-12-05 | 2019-04-05 | 吉林大学 | A kind of lithium ion battery negative material and preparation method thereof, lithium ion cell electrode piece and lithium ion battery |
| CN109935807A (en) * | 2019-02-27 | 2019-06-25 | 福建翔丰华新能源材料有限公司 | A method of it aoxidizing sub- silicon and prepares lithium ion battery negative material |
| WO2022225469A1 (en) * | 2021-04-19 | 2022-10-27 | Khon Kaen University | High-purity nanosilica and nanosilicon manufacturing process |
| CN115156239A (en) * | 2022-07-15 | 2022-10-11 | 山东邦凯新材料有限公司 | Device and processing technology for preparing high-purity silicon dioxide by continuous recovery treatment of hazardous waste silica gel |
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Application publication date: 20111123 |