CN104030290A - Method for producing nanometer silicon by adopting rice hull - Google Patents
Method for producing nanometer silicon by adopting rice hull Download PDFInfo
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- CN104030290A CN104030290A CN201410306486.1A CN201410306486A CN104030290A CN 104030290 A CN104030290 A CN 104030290A CN 201410306486 A CN201410306486 A CN 201410306486A CN 104030290 A CN104030290 A CN 104030290A
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Abstract
The invention relates to a method for producing nanometer silicone by adopting rice hull. The method for producing the nanometer silicone by adopting the rice hull comprises the following steps: carrying out heat treatment on the rice hull, so that silicon dioxide is obtained; carrying out reduction reaction on the silicon dioxide and magnesium, so that an intermediate containing the nanometer silicone, magnesium silicide, silicon dioxide and magnesium oxide is obtained; treating the intermediate with hydrochloric acid, separating filtrate containing magnesium silicate and magnesium oxide, and treating with hydrofluoric acid, filtering to remove filtrate containing silicon dioxide; rinsing products of the previous step to be neutral, and drying, so that the nanometer silicone is obtained. By applying the method for producing the nanometer silicone by adopting the rice hull, the nanometer silicone can be produced by adopting the rice hull, the rice hull can be changed into things of value, pollution to the environment when the rice hull is incinerated is reduced, production cost of the nanometer silicone is reduced, and considerable social benefit and economic benefit can be obtained; the obtained nanometer silicon material has porous structures and strong physical properties and can be applied to the fields of medicines, electronics and environmental protection.
Description
[technical field]
The present invention relates to produce the technique of nano-silicon, be specifically related to a kind of method of producing nano-silicon with rice husk.
[background technology]
China is the big country that produces rice, and the output of at present annual rice, about 200,000,000 tons of left and right, is estimated the approximately 5,000 ten thousand tons of left and right of rice husk that produce.Paddy belongs to grass, and its epidermis is hard, wherein contains silica cell, and silica cell is often full of by single silica nodule, contains abundant element silicon.The common process of rice husk approximately 10% left and right is used for doing feed, and 20% left and right recycling is used in rudimentary industrial auxiliary material, and a part of 70% is as the rear as fertilizer sources waterlogged plot of burning, and all the other are as other purposes.Some Chan Dao great districts at home, the smog that the rice husk of burning every year produces, produces and pollutes atmosphere, is also a challenge for administering haze.
Meanwhile, nano-silicon, as photoelectricity semiconductor material of new generation and high power light source material, is widely used in the circuit as IC, solar cell, the electronic applications of large-scale integrated circuit etc.The nano-silicon production method cost of prior art is higher, and the production cost that reduces nano-silicon is that electronic applications is urgently wanted the problem solving.
[summary of the invention]
One of object of the present invention is to solve the defect that in prior art, the element silicon in rice husk is wasted by major part, and rice husk is become and given up as the raw material of high added value.
Two of object of the present invention is to solve the too high problem of nano-silicon production cost in prior art.
Three of object of the present invention is to make element silicon in rice husk change nano-silicon into become possibility.
To achieve these goals, the invention provides a kind of method of producing nano-silicon with rice husk, the method comprises the following steps:
A. will after rice husk thermal treatment, obtain silicon-dioxide;
B. silicon-dioxide and magnesium are carried out to reduction reaction and obtain comprising nano-silicon, magnesium silicide, silicon-dioxide and magnesian intermediate;
C. intermediate is processed to separate through persalt and is contained magnesium silicide and magnesian filtrate, filters and removes the filtrate of containing silicon-dioxide through hydrofluoric acid treatment;
D. upper step product obtains nano-silicon through rinsing after neutral, dry.
The present invention also further provides the Optimization Technology step of aforesaid method:
Before step a, can also comprise the step of rice husk removal heavy metal.Further, the step of removal heavy metal is: rice husk is cleaned, removed its inner heavy metal through persalt pre-treatment, then rinse, be dried.Get rid of the heavy metal in rice husk, make later treating processes become comparatively simple.
Above-mentioned concentration of hydrochloric acid is preferably 1mol/L.
Described heat treatment step can operate as follows: rice husk is put into heat treatment furnace, at 750 DEG C, heat 2-5 hour.
The mass ratio of silicon-dioxide and magnesium powder is preferably silicon-dioxide: magnesium powder=1:2.3.Further, the reactions steps of silicon-dioxide and magnesium is: evenly mixed silica and magnesium reacts after mixing and within 2-4 hour, obtains described intermediate at 730 DEG C.
Intermediate and hydrochloric acid carry out centrifugation after being uniformly mixed 10～20 hours with the speed of 300 revs/min, remove and contain magnesium silicide and magnesian filtrate.
Put into the speed with 200 revs/min in the hydrofluoric acid solution of percentage concentration 1% through the intermediate of persalt processing and stir 15-20 minute, filter and remove the filtrate of containing silicon-dioxide.
Finally, the nano-silicon diameter obtaining is between 20-30 nanometer, and specific surface area is in 250-300 meters squared per gram.
By method of the present invention, what make produces nano-silicon with rice husk and becomes possibility, not only makes rice husk turn waste into wealth, and has reduced and has burned the pollution of rice husk for environment, and reduced the production cost of nano-silicon, can obtain considerable social benefit and economic interests.The nano silicon material obtaining has cavernous structure, and physical property is strong, can be applied to medicine, electronics, and field of Environment Protection.
[brief description of the drawings]
Fig. 1 prepares the image of silicon-dioxide under electron microscope by paddy;
Fig. 2 is the image of nano-silicon of the present invention under electron microscope.
[embodiment]
By concrete case study on implementation, the present invention is elaborated below, but the present invention is not limited to following examples.
Following material if no special instructions, all can be purchased from open commercial sources.
Experiment use equipment and instrument:
One of retort furnace;
One, agitator for small test;
One of compact centrifuge;
One of vacuum drying oven;
One of specific-surface area detection instrument;
One of scanning electronic microscope;
Specific implementation process is as follows:
The rice husk of 50g is put into clear water and soak two hours to remove silt and other appearance dirt settlings, after taking out, in baking oven, 80C is dried;
It is 10% that rice husk after drying is immersed to concentration, soaks 2 hours in the hydrochloric acid of the about 500ml of capacity, takes out rear with pure water cleaning, by clean remaining pickling;
Putting into the speed that retort furnace divides with 30C/ and be warmed up to 750C, be then incubated 3 hours, take out after cooling, is the silicon-dioxide of 9g left and right.
Above-mentioned silicon-dioxide and magnesium powder are evenly mixed with the ratio of 1:2.3, after the silicon-dioxide of 9g and the even mixing of the magnesium powder of 8.28g, put in airtight container, then container is put into heat treatment furnace, the temperature rise speed dividing with 40C/ reacts 4 hours to 730C, then naturally cooling, obtains nano-silicon and magnesium silicide and magnesian mixture.
It is 1ml/L that above-mentioned mixture is put into concentration, in the hydrochloric acid soln of about 600ml, under 25C temperature condition, use small test agitator to stir 12 hours, then use whizzer to carry out centrifugation to reaction solution, then filter out part magnesium silicide, remaining is part silicon-dioxide and the poroid silicon of nanometer.
Above-mentioned materials is put in the hydrofluoric acid solution that mass concentration is 1%, 400ml, under 25C temperature condition, use small test agitator to stir 20 minutes, then use whizzer to carry out centrifugation to reaction solution, remaining throw out, with after pure water filtering, is exactly nano-silicon.
Hydrochloric acid can recycle, and the heavy metal and the magnesium that are dissolved in hydrochloric acid can extract by electro-plating method, and in addition, the water of rinsing can decontamination cycle use.
The Fig. 1 obtaining from scanning electron microscope can see, the silicon-dioxide of just having handled is bulk, and the structure of crystal inside is very tight.
The Fig. 2 obtaining from scanning electron microscope can see through whole process nano-silicon internal structure after treatment even, and it is poroid to be ball, and aperture is between 20-30 nanometer.
The nano-silicon extracting from rice husk, can be used as medical intermediate, and it can absorb the drug, and at aura, district slowly discharges, and plays the effect that general medicine is difficult to performance.
It can be used as the negative material of lithium cell, and a gram appearance ratio meets or exceeds 2000mah/g, exceeds more than 3 times than common lithium cell.
It can also serve as the sensor of various gases, has a lot of use value aspect environmental protection.
The present invention has started a brand-new green energy resource pattern as one directly from the utilization of resources of agricultural wastes, from a reproducible waste resource, converts an industrial novel material to, and consequent social benefit and economic interests have greatly improved.
The above is specific embodiments of the invention; under the premise without departing from the principles of the invention; for the those of ordinary skill of being engaged in this technical scope, can also make some improvement and modification, these improve and modification all will be regarded as protection scope of the present invention.
Claims (10)
1. a method of producing nano-silicon with rice husk, is characterized in that comprising the following steps:
A. will after rice husk thermal treatment, obtain silicon-dioxide;
B. silicon-dioxide and magnesium are carried out to reduction reaction and obtain comprising nano-silicon, magnesium silicide, silicon-dioxide and magnesian intermediate;
C. intermediate is processed to separate through persalt and is contained magnesium silicide and magnesian filtrate, filters and removes the filtrate of containing silicon-dioxide through hydrofluoric acid treatment;
D. upper step product obtains nano-silicon through rinsing after neutral, dry.
2. rice husk as claimed in claim 1 is produced the method for nano-silicon, it is characterized in that also comprising the step of rice husk removal heavy metal before step a.
3. rice husk as claimed in claim 2 is produced the method for nano-silicon, it is characterized in that the step of removal heavy metal is: rice husk is cleaned, removed its inner heavy metal through persalt pre-treatment, then rinse, be dried.
4. the rice husk as described in claim 1 or 3 is produced the method for nano-silicon, it is characterized in that described concentration of hydrochloric acid is 1mol/L.
5. rice husk as claimed in claim 1 is produced the method for nano-silicon, it is characterized in that described thermal treatment is: rice husk is put into heat treatment furnace, at 750 DEG C, heat 2-5 hour.
6. rice husk as claimed in claim 1 is produced the method for nano-silicon, and the mass ratio that it is characterized in that silicon-dioxide and magnesium powder is silicon-dioxide: magnesium powder=1:2.3.
7. the rice husk as described in claim 1 or 6 is produced the method for nano-silicon, it is characterized in that the reactions steps of silicon-dioxide and magnesium is: evenly mixed silica and magnesium reacts after mixing and within 2-4 hour, obtains described intermediate at 730 DEG C.
8. rice husk as claimed in claim 1 is produced the method for nano-silicon, it is characterized in that carrying out centrifugation after described intermediate and hydrochloric acid are uniformly mixed 10～20 hours with the speed of 300 revs/min, removes and contains magnesium silicide and magnesian filtrate.
9. rice husk as claimed in claim 1 is produced the method for nano-silicon, it is characterized in that the described intermediate through persalt processing puts into the speed with 200 revs/min in the hydrofluoric acid solution of percentage concentration 1% and stir 15-20 minute, filter and remove the filtrate of containing silicon-dioxide.
10. rice husk as claimed in claim 1 is produced the method for nano-silicon, it is characterized in that the nano-silicon diameter obtaining is between 20-30 nanometer, and specific surface area is in 250-300 meters squared per gram.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104671247A (en) * | 2015-02-11 | 2015-06-03 | 武汉科技大学 | Method for preparing superfine nano-silicon by taking silicon-containing biomass as raw material as well as prepared superfine nano-silicon and application thereof |
| CN105084365A (en) * | 2015-07-17 | 2015-11-25 | 中国科学技术大学 | Preparation method for silicon nano material and application |
| CN105347346A (en) * | 2015-12-08 | 2016-02-24 | 武汉科技大学 | Method for preparing porous nanometer silicon through air auxiliary |
| CN105347347A (en) * | 2015-12-08 | 2016-02-24 | 华中科技大学 | Method for preparing three-dimensional porous nanometer silicon at low temperature through molten-salt growth method |
| CN106241812A (en) * | 2016-07-29 | 2016-12-21 | 中国科学技术大学 | The method preparing silicon nano material |
| CN106848275A (en) * | 2017-03-09 | 2017-06-13 | 湘潭大学 | A kind of preparation method of lithium ion battery negative material silica aerogel |
| CN107565118A (en) * | 2017-08-30 | 2018-01-09 | 山东大学 | A kind of preparation method of high-performance lithium ion nano-silicon negative material |
| CN110040734A (en) * | 2019-03-15 | 2019-07-23 | 深圳市动力创新科技企业（有限合伙） | A kind of nano-silicon and preparation method thereof |
| CN110402500A (en) * | 2017-01-25 | 2019-11-01 | 乔治华盛顿大学 | By Jin Teer phase low temperature high yield nano materials and composite material |
| WO2022225469A1 (en) * | 2021-04-19 | 2022-10-27 | Khon Kaen University | High-purity nanosilica and nanosilicon manufacturing process |
| CN115838183A (en) * | 2023-02-15 | 2023-03-24 | 中南大学 | Method for separating silicon and magnesium from black talc |
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| CN102249239A (en) * | 2011-06-08 | 2011-11-23 | 浙江大学 | Preparation method for preparing high-purity simple substance silicon from agricultural wastes |
| CN102259858A (en) * | 2011-06-07 | 2011-11-30 | 同济大学 | Method for preparing porous silicon by magnesiothermic reduction |
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2014
- 2014-06-30 CN CN201410306486.1A patent/CN104030290B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102259858A (en) * | 2011-06-07 | 2011-11-30 | 同济大学 | Method for preparing porous silicon by magnesiothermic reduction |
| CN102249239A (en) * | 2011-06-08 | 2011-11-23 | 浙江大学 | Preparation method for preparing high-purity simple substance silicon from agricultural wastes |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104671247A (en) * | 2015-02-11 | 2015-06-03 | 武汉科技大学 | Method for preparing superfine nano-silicon by taking silicon-containing biomass as raw material as well as prepared superfine nano-silicon and application thereof |
| CN105084365A (en) * | 2015-07-17 | 2015-11-25 | 中国科学技术大学 | Preparation method for silicon nano material and application |
| CN105347346B (en) * | 2015-12-08 | 2020-10-16 | 武汉科技大学 | Air-assisted preparation method of porous nano silicon |
| CN105347346A (en) * | 2015-12-08 | 2016-02-24 | 武汉科技大学 | Method for preparing porous nanometer silicon through air auxiliary |
| CN105347347A (en) * | 2015-12-08 | 2016-02-24 | 华中科技大学 | Method for preparing three-dimensional porous nanometer silicon at low temperature through molten-salt growth method |
| CN106241812A (en) * | 2016-07-29 | 2016-12-21 | 中国科学技术大学 | The method preparing silicon nano material |
| CN110402500A (en) * | 2017-01-25 | 2019-11-01 | 乔治华盛顿大学 | By Jin Teer phase low temperature high yield nano materials and composite material |
| CN106848275A (en) * | 2017-03-09 | 2017-06-13 | 湘潭大学 | A kind of preparation method of lithium ion battery negative material silica aerogel |
| CN107565118A (en) * | 2017-08-30 | 2018-01-09 | 山东大学 | A kind of preparation method of high-performance lithium ion nano-silicon negative material |
| CN110040734A (en) * | 2019-03-15 | 2019-07-23 | 深圳市动力创新科技企业（有限合伙） | A kind of nano-silicon and preparation method thereof |
| WO2022225469A1 (en) * | 2021-04-19 | 2022-10-27 | Khon Kaen University | High-purity nanosilica and nanosilicon manufacturing process |
| CN115838183A (en) * | 2023-02-15 | 2023-03-24 | 中南大学 | Method for separating silicon and magnesium from black talc |
| CN115838183B (en) * | 2023-02-15 | 2023-05-26 | 中南大学 | Method for separating silicon magnesium from black talc |
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