CN109052418A - A kind of preparation method of spherical nano-silicon dioxide - Google Patents
A kind of preparation method of spherical nano-silicon dioxide Download PDFInfo
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- CN109052418A CN109052418A CN201811104011.9A CN201811104011A CN109052418A CN 109052418 A CN109052418 A CN 109052418A CN 201811104011 A CN201811104011 A CN 201811104011A CN 109052418 A CN109052418 A CN 109052418A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The present invention relates to a kind of preparation methods of spherical nano-silicon dioxide, belong to technical field of nanometer material preparation.The present invention is first using Eucalyptus as raw material, it is mixed after being ground into particle with bed-silt, and micro- corruption under conditions of high temperature and humidity, obtain micro- rotten Eucalyptus particle, then through sided corona treatment after being carbonized, obtain self-control control shape template, nano silica is finally prepared using homogeneous precipitation method, and self-control control shape agent is added during the preparation process, it is calcined after preparation, finally obtains spherical nano-silicon dioxide, nano silica uniform particle diameter produced by the present invention, not easy to reunite, pattern is spherical shape, has wide application prospect.
Description
Technical field
The present invention relates to a kind of preparation methods of spherical nano-silicon dioxide, belong to technical field of nanometer material preparation.
Background technique
Nano silica is since its partial size is small, and large specific surface area, adsorption ability is strong, and surface can be big, chemical purity
Height, dispersion performance is good, has the function of special and its superior stability, reinforcing, thickening property in thermal resistance and resistance
With thixotroping shape, therefore it is widely used in rubber, plastics, ceramics, the fields such as chemical catalysis.Currently, preparing for nano material is main
There are physical method and chemical method, physical method has vacuum condensation method, physical crushing method and mechanical attrition method etc., and chemical method has
Vapour deposition process, the precipitation method, sol-gal process, microemulsion method, hydrothermal synthesis method etc..And the preparation method of nano silica
There are two kinds of dry and wet, dry method includes vapor phase method and arc process, wet process fractional precipitation method and gel method.
The precipitation method are silicates by being acidified the SiO that acquisition is loose, finely divided, is precipitated out with flocculent structure2Crystal.
The method raw material is easy to get, and production procedure is simple, and low energy consumption, small investment, but product quality is not as good as using vapor phase method and gel method
Product is good and the silica partial size that generates is inhomogenous, is easy to happen reunion, influences application prospect.
Because of a kind of uniform particle diameter of the invention, the preparation method pair of the spherical nano-silicon dioxide of controlled shape in preparation process
Technical field of nanometer material preparation has positive meaning.
Summary of the invention
Present invention mainly solves the technical issues of, for the current precipitation method prepare nano silica during titanium dioxide
Silicon shape is uncontrollable, and partial size is inhomogenous, is easy to happen reunion, influences the defect of application prospect, provides a kind of ball shaped nano two
The preparation method of silica.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of spherical nano-silicon dioxide, it is characterised in that specific preparation step are as follows:
(1) it weighs Eucalyptus and is put into 20~30min of crushing in pulverizer, sieving obtains the Eucalyptus that partial size is 3~5mm after crushing
Particle is put into greenhouse after mixing Eucalyptus particle and bed-silt, stands micro- rotten processing；
(2) to above-mentioned micro- rotten after treatment, micro- rotten Eucalyptus particle is obtained after being rinsed 3~5 times with deionized water, by above-mentioned micro- corruption
Eucalyptus particle is put into retort, under nitrogen protection heat preservation charing, obtains micro- rotten Eucalyptus charcoal；
(3) above-mentioned micro- rotten Eucalyptus charcoal is put into corona treatment equipment, sided corona treatment, it is modified to obtain corona after sided corona treatment
Micro- corruption Eucalyptus charcoal, as self-control control shape template；
(4) after sodium silicate solution, lecithin and the deionized water and the mixing of above-mentioned self-control control shape template for being 30% by mass fraction
It is put into reaction kettle, is stirred to react to obtain prefabricated solution, then ethyl acetate is added dropwise dropwise into reaction kettle；
(5) after above-mentioned ethyl acetate is added dropwise, continue to be stirred to react, cross the stainless steel that aperture is 1mm after reaction and sieve,
Obtained filter residue is put into Muffle furnace by isolated filter residue, and heat preservation calcining discharges up to spherical nano-silicon dioxide.
The mass ratio of Eucalyptus particle and bed-silt as described in step (1) is 1:5, and the temperature in greenhouse is 30~40 DEG C,
The relative air humidity in greenhouse is 60~70%, and the time for standing micro- rotten processing is 5~7 days.
The temperature of heat preservation charing described in step (2) is 200~300 DEG C, and the time for keeping the temperature charing is 1~2h.
The high-frequency ac voltage of sided corona treatment described in step (3) is 4000~5000V/m2, the time of sided corona treatment
For 1~2h.
Sodium silicate solution, lecithin and the deionized water and self-control control shape that mass fraction described in step (4) is 30%
The mass ratio of template is 1:1:2:1, and the temperature being stirred to react is 40~50 DEG C, and the time being stirred to react is 30~40min, acetic acid
The dripping quantity of ethyl ester is the 10~15% of prefabricated solution quality.
Continue described in step (5) temperature being stirred to react be 50~60 DEG C, continue the time being stirred to react be 3~
5h, the temperature for keeping the temperature calcining is 780~800 DEG C, and the time for keeping the temperature calcining is 1~2h.
The beneficial effects of the present invention are:
(1) present invention mixes after being ground into particle with bed-silt, and under conditions of high temperature and humidity first using Eucalyptus as raw material
Micro- corruption obtains micro- rotten Eucalyptus particle, through sided corona treatment after then being carbonized, self-control control shape template is obtained, finally using homogeneous
The precipitation method prepare nano silica, and self-control control shape agent is added during the preparation process, calcine after preparation, finally obtain ball
Shape nano silica, the present invention is by mixing Eucalyptus particle and bed-silt rich in microorganism, in the work of high temperature and humidity
Micro- corruption under acts on Eucalyptus particle using micro- corruption of microorganism and shows to be formed meso-hole structure, then by it is micro- it is rotten after Eucalyptus particle
Charing obtains micro- rotten Eucalyptus charcoal with meso-hole structure, most by sided corona treatment, generates a large amount of activity in micro- rotten Eucalyptus carbon surface
Hydroxyl improves the adsorptivity of micro- rotten Eucalyptus charcoal, obtains self-control control shape template and adds later using waterglass as raw material into waterglass
Enter ethyl acetate, hydrolysis occurs in waterglass for ethyl acetate, and the pH value of reaction system can be made uniform in homogeneous system
Ground reduces, and causes that localized acidity is excessively high, basicity reduces too fast phenomenon when so as to avoid being directly added into acid, can make water
The latent acid reagent of polymerisation of silicate is capable of providing more preferably reaction condition in glass, is conducive to control nano silica
The size and pattern of crystal, and the addition of natural surfactant ovum congealed fat can effectively control the molding of silica crystals,
Keep its partial size more uniform, and nano silica generated in the reaction system can immerse it by self-control control shape template absorption
In meso-hole structure abundant, particle is prevented to continue to grow up, to obtain spherical meso-porous nano grade silicon dioxide, is forged in last
During burning, making by oneself can continue to hinder the reunion of spherical nano-silicon dioxide micro- rotten Eucalyptus charcoal early period, and the two of later period calcining generation
Carbon oxide gas can make spherical nano-silicon dioxide powder bulk in volatilization process, keep spherical structure, finally obtain product,
Whole process, the shape and size tunable of nanometer titanium dioxide silicon crystal, has broad application prospects.
Specific embodiment
It weighs Eucalyptus and is put into 20~30min of crushing in pulverizer, sieving obtains the eucalyptus that partial size is 3~5mm after crushing
Eucalyptus particle and bed-silt are that be put into temperature be 30~40 DEG C after 1:5 is mixed by the wooden particle in mass ratio, relative air humidity
In 60~70% greenhouse, to stand micro- rotten processing 5~7 days；To micro- rotten after treatment, after being rinsed 3~5 times with deionized water
Micro- rotten Eucalyptus particle is obtained, above-mentioned micro- rotten Eucalyptus particle is put into retort, it is heated to 200 under nitrogen protection~
300 DEG C, heat preservation 1~2h of charing obtains micro- rotten Eucalyptus charcoal；Micro- rotten Eucalyptus charcoal is put into corona treatment equipment, in high-frequency ac
Voltage is 4000~5000V/m2Under conditions of 1~2h of sided corona treatment, the modified micro- rotten Eucalyptus of corona is obtained after sided corona treatment
Charcoal, as self-control control shape template；Be in mass ratio 1:1:2:1 be 30% by mass fraction sodium silicate solution, lecithin and go from
It is put into reaction kettle after sub- water and the mixing of above-mentioned self-control control shape template, is stirred to react 30~40min at 40~50 DEG C and obtains
Prefabricated solution, then the ethyl acetate of prefabricated solution quality 10~15% is added dropwise into reaction kettle dropwise；After ethyl acetate is added dropwise,
Continue to be stirred to react 3~5h at 50~60 DEG C, crosses the stainless steel that aperture is 1mm after reaction and sieve, isolated filter residue will
Obtained filter residue is put into Muffle furnace, is warming up to 780~800 DEG C, heat preservation 1~2h of calcining with 3~5 DEG C/min rate program, discharging
Up to spherical nano-silicon dioxide.
It weighing Eucalyptus and is put into pulverizer and crush 20min, sieving obtains the Eucalyptus particle that partial size is 3mm after crushing,
It is in mass ratio that be put into temperature be 30 DEG C after 1:5 is mixed by Eucalyptus particle and bed-silt, the greenhouse that relative air humidity is 60%
In, stand micro- rotten processing 5 days；To micro- rotten after treatment, micro- rotten Eucalyptus particle is obtained after being rinsed 3 times with deionized water, it will be upper
It states micro- rotten Eucalyptus particle to be put into retort, is heated to 200 DEG C under nitrogen protection, heat preservation charing 1h obtains micro- rotten eucalyptus
Charcoal；Micro- rotten Eucalyptus charcoal is put into corona treatment equipment, is 4000V/m in high-frequency ac voltage2Under conditions of sided corona treatment
1h obtains the modified micro- rotten Eucalyptus charcoal of corona, as self-control control shape template after sided corona treatment；It is in mass ratio that 1:1:2:1 will
Reaction is put into after sodium silicate solution, lecithin and deionized water and the mixing of above-mentioned self-control control shape template that mass fraction is 30%
In kettle, it is stirred to react 30min at 40 DEG C and obtains prefabricated solution, then the acetic acid of prefabricated solution quality 10% is added dropwise dropwise into reaction kettle
Ethyl ester；After ethyl acetate is added dropwise, continue to be stirred to react 3h at 50 DEG C, crossing aperture after reaction is the stainless of 1mm
Obtained filter residue is put into Muffle furnace, is warming up to 780 DEG C with 3 DEG C/min rate program, heat preservation is forged by steel sieve, isolated filter residue
1h is burnt, is discharged up to spherical nano-silicon dioxide.
It weighing Eucalyptus and is put into pulverizer and crush 25min, sieving obtains the Eucalyptus particle that partial size is 4mm after crushing,
It is in mass ratio that be put into temperature be 35 DEG C after 1:5 is mixed by Eucalyptus particle and bed-silt, the greenhouse that relative air humidity is 65%
In, stand micro- rotten processing 6 days；To micro- rotten after treatment, micro- rotten Eucalyptus particle is obtained after being rinsed 4 times with deionized water, it will be upper
It states micro- rotten Eucalyptus particle to be put into retort, is heated to 250 DEG C under nitrogen protection, heat preservation charing 1h obtains micro- rotten eucalyptus
Charcoal；Micro- rotten Eucalyptus charcoal is put into corona treatment equipment, is 4500V/m in high-frequency ac voltage2Under conditions of sided corona treatment
2h obtains the modified micro- rotten Eucalyptus charcoal of corona, as self-control control shape template after sided corona treatment；It is in mass ratio that 1:1:2:1 will
Reaction is put into after sodium silicate solution, lecithin and deionized water and the mixing of above-mentioned self-control control shape template that mass fraction is 30%
In kettle, it is stirred to react 35min at 45 DEG C and obtains prefabricated solution, then the acetic acid of prefabricated solution quality 13% is added dropwise dropwise into reaction kettle
Ethyl ester；After ethyl acetate is added dropwise, continue to be stirred to react 4h at 55 DEG C, crossing aperture after reaction is the stainless of 1mm
Obtained filter residue is put into Muffle furnace, is warming up to 790 DEG C with 4 DEG C/min rate program, heat preservation is forged by steel sieve, isolated filter residue
2h is burnt, is discharged up to spherical nano-silicon dioxide.
It weighing Eucalyptus and is put into pulverizer and crush 30min, sieving obtains the Eucalyptus particle that partial size is 5mm after crushing,
It is in mass ratio that be put into temperature be 40 DEG C after 1:5 is mixed by Eucalyptus particle and bed-silt, the greenhouse that relative air humidity is 70%
In, stand micro- rotten processing 7 days；To micro- rotten after treatment, micro- rotten Eucalyptus particle is obtained after being rinsed 5 times with deionized water, it will be upper
It states micro- rotten Eucalyptus particle to be put into retort, is heated to 300 DEG C under nitrogen protection, heat preservation charing 2h obtains micro- rotten eucalyptus
Charcoal；Micro- rotten Eucalyptus charcoal is put into corona treatment equipment, is 5000V/m in high-frequency ac voltage2Under conditions of sided corona treatment
2h obtains the modified micro- rotten Eucalyptus charcoal of corona, as self-control control shape template after sided corona treatment；It is in mass ratio that 1:1:2:1 will
Reaction is put into after sodium silicate solution, lecithin and deionized water and the mixing of above-mentioned self-control control shape template that mass fraction is 30%
In kettle, it is stirred to react 40min at 50 DEG C and obtains prefabricated solution, then the acetic acid of prefabricated solution quality 15% is added dropwise dropwise into reaction kettle
Ethyl ester；After ethyl acetate is added dropwise, continue to be stirred to react 5h at 60 DEG C, crossing aperture after reaction is the stainless of 1mm
Obtained filter residue is put into Muffle furnace, is warming up to 800 DEG C with 5 DEG C/min rate program, heat preservation is forged by steel sieve, isolated filter residue
2h is burnt, is discharged up to spherical nano-silicon dioxide.
Reference examples keep other raw materials constant, do not add self-control control shape template, prepare nano silica by same steps,
And in this, as reference examples；
Performance detection, detection knot are carried out to the nano silica in spherical nano-silicon dioxide produced by the present invention and reference examples
Fruit is as shown in table 1:
1 performance test results of table
| Performance test results | Example 1 | Example 2 | Example 3 | Reference examples |
| Particle size range (nm) | 30~50 | 30~50 | 30~50 | 100~1000 |
| Pattern | It is spherical, non-aggregated | It is spherical, non-aggregated | It is spherical, non-aggregated | Pattern is uneven, reunites |
Nano silica uniform particle diameter produced by the present invention, not easy to reunite it can be seen from testing result in upper table, and pattern is
Spherical shape has wide application prospect.
Claims (6)
1. a kind of preparation method of spherical nano-silicon dioxide, it is characterised in that specific preparation step are as follows:
(1) it weighs Eucalyptus and is put into 20~30min of crushing in pulverizer, sieving obtains the Eucalyptus that partial size is 3~5mm after crushing
Particle is put into greenhouse after mixing Eucalyptus particle and bed-silt, stands micro- rotten processing；
(2) to above-mentioned micro- rotten after treatment, micro- rotten Eucalyptus particle is obtained after being rinsed 3~5 times with deionized water, by above-mentioned micro- corruption
Eucalyptus particle is put into retort, under nitrogen protection heat preservation charing, obtains micro- rotten Eucalyptus charcoal；
(3) above-mentioned micro- rotten Eucalyptus charcoal is put into corona treatment equipment, sided corona treatment, it is modified to obtain corona after sided corona treatment
Micro- corruption Eucalyptus charcoal, as self-control control shape template；
(4) after sodium silicate solution, lecithin and the deionized water and the mixing of above-mentioned self-control control shape template for being 30% by mass fraction
It is put into reaction kettle, is stirred to react to obtain prefabricated solution, then ethyl acetate is added dropwise dropwise into reaction kettle；
(5) after above-mentioned ethyl acetate is added dropwise, continue to be stirred to react, cross the stainless steel that aperture is 1mm after reaction and sieve,
Obtained filter residue is put into Muffle furnace by isolated filter residue, and heat preservation calcining discharges up to spherical nano-silicon dioxide.
2. a kind of preparation method of spherical nano-silicon dioxide according to claim 1, it is characterised in that: in step (1)
The mass ratio of the Eucalyptus particle and bed-silt is 1:5, and the temperature in greenhouse is 30~40 DEG C, the relative air humidity in greenhouse
It is 60~70%, the time for standing micro- rotten processing is 5~7 days.
3. a kind of preparation method of spherical nano-silicon dioxide according to claim 1, it is characterised in that: in step (2)
The temperature of the heat preservation charing is 200~300 DEG C, and the time for keeping the temperature charing is 1~2h.
4. a kind of preparation method of spherical nano-silicon dioxide according to claim 1, it is characterised in that: in step (3)
The high-frequency ac voltage of the sided corona treatment is 4000~5000V/m2, the time of sided corona treatment is 1~2h.
5. a kind of preparation method of spherical nano-silicon dioxide according to claim 1, it is characterised in that: in step (4)
The mass ratio of sodium silicate solution, lecithin and deionized water and self-control control shape template that the mass fraction is 30% is 1:
1:2:1, the temperature being stirred to react are 40~50 DEG C, and the time being stirred to react is 30~40min, and the dripping quantity of ethyl acetate is pre-
The 10~15% of liquid quality processed.
6. a kind of preparation method of spherical nano-silicon dioxide according to claim 1, it is characterised in that: in step (5)
The temperature for continuing to be stirred to react is 50~60 DEG C, and continuing the time being stirred to react is 3~5h, and the temperature for keeping the temperature calcining is
780~800 DEG C, the time for keeping the temperature calcining is 1~2h.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107029657A (en) * | 2017-05-14 | 2017-08-11 | 刘滨 | A kind of preparation method of porous high-temperature carbon dioxide absorbing material |
| CN107200332A (en) * | 2017-06-07 | 2017-09-26 | 常州诺澜复合材料有限公司 | A kind of preparation method of nano silicon |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107029657A (en) * | 2017-05-14 | 2017-08-11 | 刘滨 | A kind of preparation method of porous high-temperature carbon dioxide absorbing material |
| CN107200332A (en) * | 2017-06-07 | 2017-09-26 | 常州诺澜复合材料有限公司 | A kind of preparation method of nano silicon |
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