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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- elemental silicon
- powder
- agricultural waste
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- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 41
- 239000010703 silicon Substances 0.000 title claims abstract description 41
- 239000002154 agricultural waste Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims description 11
- 239000000126 substance Substances 0.000 title description 2
- 239000000843 powder Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 36
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 11
- 239000001301 oxygen Substances 0.000 claims description 11
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 7
- 235000007164 Oryza sativa Nutrition 0.000 claims description 7
- 240000008042 Zea mays Species 0.000 claims description 7
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 7
- 235000009566 rice Nutrition 0.000 claims description 7
- 239000010902 straw Substances 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 239000003638 chemical reducing agent Substances 0.000 claims description 6
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 5
- 235000005822 corn Nutrition 0.000 claims description 5
- 239000010903 husk Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 235000013399 edible fruits Nutrition 0.000 claims description 4
- 241000196324 Embryophyta Species 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 238000012271 agricultural production Methods 0.000 claims 1
- 239000005416 organic matter Substances 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 16
- 239000002994 raw material Substances 0.000 abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 6
- 230000002829 reductive effect Effects 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000000197 pyrolysis Methods 0.000 abstract description 3
- 239000000377 silicon dioxide Substances 0.000 abstract description 3
- 238000010306 acid treatment Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 10
- 238000002156 mixing Methods 0.000 description 9
- 238000001816 cooling Methods 0.000 description 7
- 241000209094 Oryza Species 0.000 description 6
- 239000004411 aluminium Substances 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 235000016383 Zea mays subsp huehuetenangensis Nutrition 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 235000009973 maize Nutrition 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 235000015099 wheat brans Nutrition 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 208000032170 Congenital Abnormalities Diseases 0.000 description 1
- 206010010356 Congenital anomaly Diseases 0.000 description 1
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 1
- 239000012773 agricultural material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007698 birth defect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- YTHCQFKNFVSQBC-UHFFFAOYSA-N magnesium silicide Chemical compound [Mg]=[Si]=[Mg] YTHCQFKNFVSQBC-UHFFFAOYSA-N 0.000 description 1
- 229910021338 magnesium silicide Inorganic materials 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- -1 poly(oxygen-silicon) Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
本发明公开了一种从农业废弃物制备高纯单质硅的制备方法。通过简单的两个步骤：首先将农业废弃物通过热解成为多孔二氧化硅粉体；随后通过酸处理、金属热反应等去除其中的杂质并将二氧化硅还原成为单质硅。由于农业废弃物经过热解后结构松散，其中的杂质易去除，因此所得单质硅的纯度在99%以上，有利于直接应用或进行进一步加工处理。本发明提出的从农业废弃物制备高纯单质硅的方法，原材料成本低廉，工艺流程简单，具有极强的经济价值和应用前景。The invention discloses a method for preparing high-purity elemental silicon from agricultural waste. Through two simple steps: first, the agricultural waste is pyrolyzed into porous silica powder; then, impurities are removed through acid treatment, metal thermal reaction, etc., and the silica is reduced to elemental silicon. Since the structure of agricultural waste is loose after pyrolysis, the impurities in it are easy to remove, so the purity of the obtained elemental silicon is more than 99%, which is conducive to direct application or further processing. The method for preparing high-purity elemental silicon from agricultural wastes proposed by the invention has low cost of raw materials, simple process flow, and strong economic value and application prospect.
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)
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|---|---|---|---|
| CN 201110152177 CN102249239A (en) | 2011-06-08 | 2011-06-08 | Preparation method for preparing high-purity simple substance silicon from agricultural wastes |
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|---|---|---|---|
| CN 201110152177 CN102249239A (en) | 2011-06-08 | 2011-06-08 | Preparation method for preparing high-purity simple substance silicon from agricultural wastes |
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| Publication Number | Publication Date |
|---|---|
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ID=44976878
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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 |
| 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 |
| CN117865691A (en) * | 2024-01-23 | 2024-04-12 | 云南贵金属实验室有限公司 | A low-oxygen-content silicon nitride powder and its aluminothermic reduction method and application |
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 (10)
| 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 |
| CN117865691A (en) * | 2024-01-23 | 2024-04-12 | 云南贵金属实验室有限公司 | A low-oxygen-content silicon nitride powder and its aluminothermic reduction method and application |
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Application publication date: 20111123 |