CN106115720B - A kind of method that utilization rice hull ash prepares nano silicon - Google Patents
A kind of method that utilization rice hull ash prepares nano silicon Download PDFInfo
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- CN106115720B CN106115720B CN201610665873.3A CN201610665873A CN106115720B CN 106115720 B CN106115720 B CN 106115720B CN 201610665873 A CN201610665873 A CN 201610665873A CN 106115720 B CN106115720 B CN 106115720B
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/126—Preparation of silica of undetermined type
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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Abstract
The present invention relates to silica production technical field, more particularly to a kind of method that utilization rice hull ash prepares nano silicon.Method and step is as follows:(1) preparation of sodium metasilicate;(2) preparation of nano silicon:Sodium silicate solution described in step (1) is warming up to 70 90 DEG C, is pumped in the spray gun of spray drying tower, while being passed through CO2And air gas mixture, the CO2With the pressure of air gas mixture:1.8 3.0MPa, temperature:80 100 DEG C, flow velocity is:1 15L/min, the sodium silicate solution is 1g with the mass volume ratio of the mixed gas:2‑8L;The slurry of reaction comes together in reaction tower bottom, and slurry is put into sedimentation in subsider, supernatant liquor is collected, and is rinsed through water and is precipitated to pH in neutrality, after precipitation is spray-dried, produces nano silicon, and yield is 85 95%.Device manufacturing process is simple, low cost, it is easy to industrialize, easy to maintenance.
Description
Technical field
The present invention relates to silica production technical field, more particularly to one kind nano silicon is prepared using rice hull ash
Method.
Background technology
White carbon is broadly divided into precipitated silica and fume colloidal silica by production method.Precipitated silica is divided into again
Traditional precipitated silica and special precipitation white carbon, the former refers to sulfuric acid, hydrochloric acid, CO2It is base stock with waterglass
The silica of production, the latter refers to use high-gravity technology, sol-gel process, chemical crystal method, second-crystallized method or anti-phase
The silica of the specific process such as micelle microemulsion liquid method production.Most domestic manufacturing enterprise uses the precipitation method, but the precipitation method are white
Carbon black does not actually reach nanoscale, and performance is also far unable to catch up with gas-phase silica.Fume colloidal silica, is by halogenated silanes (four
Silicon chloride, methyl trichlorosilane etc.) hydrolyzed in thermal-flame and the amorphous silica of generation, its composition can use SiO2·
nH20 represents, wherein nH2O is present in the form of surface hydroxyl.Product fineness made from vapor phase method is high, but process conditions are harsh,
Production cost is higher.Dissociating method is technically feasible, can also obtain preferable economic benefit, but technological process is complicated so that its
It is restricted in the industrial production.And though the properties of product of liquid-phase precipitation method production are good not as vapor phase method, production cost is low, and
Its performance can also meet perhaps many application requirements, thus receive suitable attention.The domestic production in white carbon at present
All there is flow complexity, operational control condition in technique study harsh, the shortcomings of production cost is of a relatively high.In addition, routine side
Product quality indicator is made from method:Pore volume 0.4cm3/g-1.8cm3/ g, BET specific surface area 130m2/g-300m2/ g, average hole
Footpath 180A-300A, DBP absorption value 2.0ml/g-3.0ml/g, particle diameter distribution D50:2.0 μm -10.0 μm, because of pore volume and oil factor
Than relatively low, impurity content is high, and the coating of production haves the shortcomings that low extinction performance, poor transparency, easy xanthochromia.
Therefore, development technology flow is simple, operating flexibility had not only had the advantages that greatly vapor phase method product but with liquid phase method into
The method of background has greater significance.
Being used for the equipment of nano silicon synthesis in currently available technology mainly has:
1st, interval bubble type reaction tower:Reaction solution is added in tower, certain liquid level is kept, CO is passed through by bottom of towe2Gas, to
Upper bubbling carries out reaction generation nano silicon.This equipment energy consumption is higher, CO2Gas consumption is big, and the reaction time is longer,
Generally reaction was at 2-4 hours, and the more difficult control of process conditions, product granularity is uneven, and particle diameter is larger, during the course of the reaction easily production
Raw parcel phenomenon, ultimately results in the product accumulation of salt in the surface soil, influences product quality, and the nano silicon product of generation easily blocks gas
Outlet.
2nd, high-speed stirred formula reaction tower:Reaction liquid is added in tower, CO is passed through2Gas, is stirred by high speed agitator,
Generate the nano silicon compared with small particle.This equipment energy consumption is higher, and equipment is complicated, easily produces during the course of the reaction solidifying
Glue so that need powerful stirring, and the nano silicon product of generation easily blocks gas vent.
3rd, roaster:Rice husk is added into roaster, silica is obtained by combusting rice hull.Although this equipment can reach
To burning, abundant, uniform, efficiency high, temperature control are accurate, but this equipment can produce substantial amounts of dioxy in combusting rice hull
Change carbon gas, environment is polluted.
The content of the invention
The invention aims to solve shortcoming present in prior art, and a kind of two fluid sprays method proposed is given birth to
Produce the device and method of nano silicon.
To achieve these goals, present invention employs following technical scheme:
A kind of method that utilization rice hull ash prepares nano silicon, method and step is as follows:
(1) preparation of sodium metasilicate:
It is 1 by rice hull ash, aqueous slkali foundation mass ratio:2-30 ratio uniform mixing, is placed in digester(-tor), digester(-tor) liter
Temperature is to 85-120 DEG C, and reaction stops heating after 1.5-5 hour, is cooled to room temperature, is transferred to mortar-trough, then through Filter Press,
Precipitation, is made sodium silicate solution, the Baume degrees of sodium silicate solution is 45 degree;
(2) preparation of nano silicon:
Sodium silicate solution described in step (1) is warming up to 70-90 DEG C, is pumped in the spray gun of spray drying tower, leads to simultaneously
Enter CO2And air gas mixture, the CO2With the pressure of air gas mixture:1.8-3.0MPa, temperature:80-100 DEG C, flow velocity
For:1-15L/min, the sodium silicate solution is 1g with the mass volume ratio of the mixed gas:2-8L;Rinse and be precipitated to through water
PH after precipitation is spray-dried, produces nano silicon, yield is 85-95% in neutrality.
Preferentially, in the step (2) provided with spray woods head in spray drying tower, intermittent shower is pure during reaction is carried out
Water, intermittent time:5-20min.Under shower water is by automatic spray in spray drying tower, slurry comes together in reaction tower bottom, will
Slurry is put into subsider and settled,
Preferentially, it is additionally provided with the spray drying tower in the step (2) and scrapes production device.
Preferentially, rice hull ash, aqueous slkali are 1 according to mass ratio in the step (1):5-15.
Preferentially, the aqueous slkali in the step (1) is the one or more in NaOH, potassium hydroxide, potassium carbonate.
Preferentially, the concentration of the aqueous slkali in the step (1) is 1-50g/ml.
Preferentially, CO in step (2) mixed gas2Volume ratio with air is 1:1-15.
By waterglass in spraying reaction tower by CO2Droplet of uniform size is dispersed into air gas mixture air-flow, is made
It must react uniform, reaction is quick.
The present invention compared with prior art, the advantage of the invention is that:
1st, the reaction tower can be carried out at ambient pressure, without power agitating device, reduce power consumption.
2nd, it is distributed in reaction tower on a spray gun, spray gun and is dispersed with liquid fluid outlet, the sleeve ring that liquid passes through spray gun
Gap and liquid fluid export to be formed inside liquid stream, spray gun by high speed CO2And air gas mixture, liquid is split into droplet,
The droplet reaction center that carbon dioxide atmosphere is surrounded is formed in reactor so that gas-liquid contact face is big, CO2Utilization rate is high, raw
Into product cut size it is small, specific surface area is big.
3rd, spray equipment is provided with the top of reaction tower, spray equipment sprayed a water every 5-20 minutes, 10 points of spray every time
Clock, the silicon dioxide gel generated after reaction can be drenched be delivered to wash mill into the convergence of reaction tower bottom together, then by pump;
The device make it that silicon dioxide gel will not block pipeline after reaction, it is easier to which continuous production, energy consumption is small.
4th, by being not easily blocked from air inlet pipe in air inlet inside spray gun, reaction tower, being normally carried out for production is conducive to.So that
Reaction tower can be produced continuously, equipment operation stable.
5th, device manufacturing process is simple, low cost, it is easy to industrialize, easy to maintenance.
6th, reaction tower middle top is provided with CO2Exhaust gas loop exit so that CO2It can recycle, shorten anti-
Between seasonable, production efficiency is improved, loss and atmosphere pollution is reduced.
Brief description of the drawings
Fig. 1 is the production process schematic diagram of the present invention.
Fig. 2 is that the two fluid spray methods used in the inventive method produce the reaction process flow of silica.
Fig. 3 is that the two fluid spray methods used in the inventive method produce the reaction tower and spray gun top profile of silica
Figure.
Fig. 4 is that the embodiment of the present invention 1 directly takes out the typical XRD of product after product drying after reaction tower reacts and spread out
Penetrate.
Fig. 5 is the transmission electron microscope picture that the embodiment of the present invention 1 directly takes out product after product drying after reaction tower reacts.
Fig. 6 is the typical XRD diffraction of the spray-dried rear product of product prepared by the embodiment of the present invention 2.
Fig. 7 is the transmission electron microscope picture of the spray-dried rear product of product prepared by the embodiment of the present invention 2.
Fig. 8 is the typical XRD diffraction of the spray-dried rear product of product prepared by the embodiment of the present invention 3.
Fig. 9 is the transmission electron microscope picture of the spray-dried rear product of product prepared by the embodiment of the present invention 3.
In figure:1 spraying reaction tower, 2 spray guns, 3 scraping devices, 4 inner tubes, 5 sleeve pipes, the outlet of 6 liquid fluids, 7 carbon dioxide,
Air gas mixture entrance, 8 spray heads, the outlet of 9 circulation of tail gas.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.
A kind of reference picture 1-3, two fluid sprays method produces the device of nano silicon, including spraying reaction tower 1, spraying
Reaction tower 1 includes spray gun 2, silicic acid sodium pump, electrical control cabinet, exhaust fan, scraping device 3, compression carbon dioxide storage tank, air
Compressor, compression carbon dioxide and air gas mixture storage tank, spray gun 2 are arranged on the top of spraying reaction tower 1, and spray gun 2 includes
Inner tube 4 and the sleeve pipe 5 being arranged on outside inner tube 4, inner tube 4 form inside and outside two fluid passages with sleeve pipe 5.
Sleeve pipe annular space is formed between inner tube 4 and sleeve pipe 5, the top in spraying reaction tower 1 is provided with spray head 8, spray gun 2
The liquid that top is provided with liquid fluid outlet 6, sleeve pipe annular space forms small thread, two by the liquid fluid outlet 6 on spray gun 2
Carbonoxide and air gas mixture are exported by inner tube by spray gun 2 to be sprayed at a high speed, and three-dimensional aerodynamic-laid web is formed in the exit of spray gun 2 will
Liquid is atomized into different size of droplet, and the aperture of liquid fluid outlet 6 is the liquid fluid outlet 6 on 1mm, the top of spray gun 2
Distribution density be 4mm2One hole, the middle part of spray gun 2 is provided with carbon dioxide, air gas mixture entrance 7, spraying reaction tower 1
Middle part be provided with circulation of tail gas outlet 9, spraying reaction tower 1 is provided with tail gas recycling device at middle part, and scraping device 3 sets
In the bottom of spraying reaction tower 1.
A kind of production method processed of the device of two fluid sprays method production nano silicon of the present invention is as follows:
Embodiment 1
A kind of method that utilization rice hull ash prepares nano silicon, specific method step is as follows:
(1) preparation of sodium metasilicate:
It is 1 by rice hull ash, aqueous slkali foundation mass ratio:20 ratio uniform mixing, is placed in digester(-tor), digester(-tor) heating
To 85- DEG C, reaction stops heating after 1.5 hours, is cooled to room temperature, is transferred to mortar-trough, then through Filter Press, precipitation, system
Sodium silicate solution is obtained, the Baume degrees of sodium silicate solution is 45 degree;
(2) preparation of nano silicon:
Sodium silicate solution described in step (1) is warming up to 70 DEG C, is pumped in the spray gun of spray drying tower, is passed through simultaneously
CO2 and air gas mixture, the CO2With the pressure of air gas mixture:1.8MPa, temperature:80 DEG C, flow velocity is:1L/min,
The sodium silicate solution is 1g with the mass volume ratio of the mixed gas:2L;The slurry of reaction comes together in reaction tower bottom, will
Slurry is put into sedimentation in subsider, collects supernatant liquor, and it is in neutrality to be rinsed through water and be precipitated to pH, after precipitation is spray-dried, i.e.,
Nano silicon is obtained, yield is 85%.
Provided with spray woods head in spray drying tower in the step (2), intermittent shower pure water in reaction progress, during interval
Between:5min.
It is additionally provided with spray drying tower in the step (2) and scrapes production device.
Step (1) rice hull ash, aqueous slkali are 1 according to mass ratio:5.
The aqueous slkali of the step (1) is NaOH.
The concentration of the aqueous slkali of the step (1) is 1g/ml.
The volume ratio of CO2 and air is 1 in step (2) mixed gas:1.
Application of the prepared nano silicon in food additives.
Embodiment 2
A kind of method that utilization rice hull ash prepares nano silicon, specific method step is as follows:
(1) preparation of sodium metasilicate:
It is 1 by rice hull ash, aqueous slkali foundation mass ratio:30 ratio uniform mixing, is placed in digester(-tor), digester(-tor) heating
To 120 DEG C, reaction stops heating after 5 hours, is cooled to room temperature, is transferred to mortar-trough, then through Filter Press, precipitation, be made
Sodium silicate solution, the Baume degrees of sodium silicate solution is 45 degree;
(2) preparation of nano silicon:
Sodium silicate solution described in step (1) is warming up to 90 DEG C, is pumped in the spray gun of spray drying tower, is passed through simultaneously
CO2 and air gas mixture, the CO2With the pressure of air gas mixture:3.0MPa, temperature:100 DEG C, flow velocity is:15L/
Min, the sodium silicate solution is 1g with the mass volume ratio of the mixed gas:8L;The slurry of reaction comes together in reaction tower bottom
Portion, slurry is put into subsider and settled, and collects supernatant liquor, is rinsed through water and is precipitated to pH in neutrality, precipitated spray-dried
Afterwards, nano silicon is produced, yield is 95%.
Provided with spray woods head in spray drying tower in the step (2), intermittent shower pure water in reaction progress, during interval
Between:20min.
It is additionally provided with spray drying tower in the step (2) and scrapes production device.
Step (1) rice hull ash, aqueous slkali are 1 according to mass ratio:15.
The aqueous slkali of the step (1) is in potassium carbonate.
The concentration of the aqueous slkali of the step (1) is 50g/ml.
The volume ratio of CO2 and air is 1 in step (2) mixed gas:15.
Application of the prepared nano silicon in tire.
Embodiment 3
A kind of method that utilization rice hull ash prepares nano silicon, specific method step is as follows:
(1) preparation of sodium metasilicate:
It is 1 by rice hull ash, aqueous slkali foundation mass ratio:18 ratio uniform mixing, is placed in digester(-tor), digester(-tor) heating
To 110 DEG C, reaction stops heating after 3.5 hours, is cooled to room temperature, is transferred to mortar-trough, then through Filter Press, precipitation, system
Sodium silicate solution is obtained, the Baume degrees of sodium silicate solution is 45 degree;
(2) preparation of nano silicon:
Sodium silicate solution described in step (1) is warming up to 85 DEG C, is pumped in the spray gun of spray drying tower, is passed through simultaneously
CO2 and air gas mixture, the CO2With the pressure of air gas mixture:2.5MPa, temperature:95 DEG C, flow velocity is:12L/
Min, the sodium silicate solution is 1g with the mass volume ratio of the mixed gas:6.5L;The slurry of reaction comes together in reaction tower
Bottom, slurry is put into subsider and settled, and collects supernatant liquor, is rinsed through water and is precipitated to pH in neutrality, precipitation is dry through spraying
After dry, nano silicon is produced, yield is 85-95%.
Provided with spray woods head in spray drying tower in the step (2), intermittent shower pure water in reaction progress, during interval
Between:18min.
It is additionally provided with spray drying tower in the step (2) and scrapes production device.
Step (1) rice hull ash, aqueous slkali are 1 according to mass ratio:12.
The aqueous slkali of the step (1) is potassium hydroxide.
The concentration of the aqueous slkali of the step (1) is 45g/ml.
The volume ratio of CO2 and air is 1 in step (2) mixed gas:13.5.
Application of the prepared nano silicon in food additives.
Surface area of the present invention is determined using full-automatic specific surface area and pore analysis instrument, model U.S. Micromeritics
ASAP 2020M+CM.Measurement result is as follows:
The inventive method of table 1 prepares its surface product
Silica product made from the embodiment 1 of table 2 is contrasted with control sample (U.S. ED3) technical target of the product
The foregoing is intended to be a preferred embodiment of the present invention, but protection scope of the present invention is not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent or change, should all be included within the scope of the present invention.
Claims (7)
1. a kind of method that utilization rice hull ash prepares nano silicon, it is characterised in that:Method and step is as follows:
(1)The preparation of sodium metasilicate:
It is 1 by rice hull ash, aqueous slkali foundation mass ratio:2-30 ratio uniform mixing, is placed in digester(-tor), digester(-tor) is warming up to
85-120 DEG C, reaction stops heating after 1.5-5 hour, is cooled to room temperature, is transferred to mortar-trough, then through Filter Press, sink
Form sediment, sodium silicate solution is made, the Baume degrees of the sodium silicate solution is 15-60 degree;
(2)The preparation of nano silicon:
Step(1)Described sodium silicate solution is warming up to 70-90 DEG C, is pumped in the spray gun of spraying reaction tower, while being passed through CO2
And air gas mixture, the CO2With the pressure of air gas mixture:1.8-3.0MPa, temperature:80-100 DEG C, flow velocity is:1-
15L/min, the sodium silicate solution is 1g with the mass volume ratio of the mixed gas:2-8L;The slurry of reaction comes together in instead
Tower bottom is answered, slurry is put into subsider and settled, supernatant liquor is collected, is rinsed through water and is precipitated to pH in neutrality, precipitation is through spray
After mist is dried, nano silicon is produced, yield is 85-95%;
The spraying reaction tower includes the top that spray gun, the spray gun are arranged on spraying reaction tower, the spray gun include inner tube and
The sleeve pipe outside inner tube is arranged on, inner tube forms inside and outside two fluid passages with sleeve pipe;Sleeve pipe is formed between said inner tube and sleeve pipe
The liquid being provided with the top of annular space, the spray gun in liquid fluid outlet, described sleeve pipe annular space passes through the liquid flow on spray gun
Body is exported to form small thread, and carbon dioxide and air gas mixture are sprayed at a high speed by inner tube by the lance outlet, described
Three-dimensional aerodynamic-laid web is formed at lance outlet and atomizes the liquid into different size of droplet, the aperture of liquid fluid outlet is 1mm, institute
The distribution density for stating the liquid fluid outlet at the top of spray gun is 4mm2One hole, the middle part of the spray gun provided with carbon dioxide,
Circulation of tail gas outlet is provided with the middle part of air gas mixture entrance, the spraying reaction tower, the spraying reaction tower is at middle part
Provided with tail gas recycling device.
2. the method that utilization rice hull ash according to claim 1 prepares nano silicon, it is characterised in that:The step
(2)In spraying reaction tower in provided with spray woods head, reaction carry out in intermittent shower pure water, intermittent time:5-20min.
3. the method that utilization rice hull ash according to claim 1 prepares nano silicon, it is characterised in that:The step
(2)In spraying reaction tower in be additionally provided with and scrape production device.
4. the method for preparing nano silicon according to the utilization rice hull ash described in claim 1, it is characterised in that:The step
(1)Rice hull ash, aqueous slkali are 1 according to mass ratio:5-15.
5. the method for preparing nano silicon according to the utilization rice hull ash described in claim 1, it is characterised in that:The step
(1)Aqueous slkali be NaOH, potassium hydroxide, potassium carbonate in one or more.
6. the method for preparing nano silicon according to the utilization rice hull ash described in claim 1, it is characterised in that:The step
(1)Aqueous slkali concentration be 1-50g/ml.
7. the method that utilization rice hull ash according to claim 1 prepares nano silicon, it is characterised in that:The step
(2)CO in mixed gas2Volume ratio with air is 1:1-15.
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CN110028074B (en) * | 2019-04-19 | 2021-08-27 | 清华大学 | Preparation method of spherical silicon dioxide |
CN110294480A (en) * | 2019-07-19 | 2019-10-01 | 四川微松新材料有限公司 | A kind of liquid phase method white carbon black and preparation method thereof |
CN111170324A (en) * | 2020-01-21 | 2020-05-19 | 张战军 | Method for preparing light high-whiteness calcium silicate micro powder by using rice hull ash |
CN113060738B (en) * | 2021-03-22 | 2022-10-21 | 哈尔滨工业大学 | Preparation of rice hull source functional carbon based on ammonia method carbon capture and nano SiO 2 Synthesis method |
CN117361548B (en) * | 2023-09-11 | 2024-05-14 | 平邑中联水泥有限公司 | Method for preparing modified hydrophilic nano silicon dioxide by utilizing straw, product and ultra-high performance concrete |
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