CN103172076B - Preparation method for silicon oxide nano-particles - Google Patents
Preparation method for silicon oxide nano-particles Download PDFInfo
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- CN103172076B CN103172076B CN201310102431.4A CN201310102431A CN103172076B CN 103172076 B CN103172076 B CN 103172076B CN 201310102431 A CN201310102431 A CN 201310102431A CN 103172076 B CN103172076 B CN 103172076B
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Abstract
The invention discloses a preparation method for silicon oxide nano-particles, which comprises the following steps of preparing organic solution of alkoxy silane with an organic solvent; adding acid into the organic solution of the alkoxy silane and then putting into a microwave chemical reactor for reacting for 2-30 minutes so as to obtain organic solution of acidic alkoxy silane, wherein the temperature is 30 DEG C-180 DEG C, and the speed of stirring is 100rpm per minute-2000rpm per minute; adding surface modifier into the organic solution of the acidic alkoxy silane and then putting into the microwave chemical reactor for reacting for 2-30 minutes, wherein the temperature is 30 DEG C-180 DEG C, and the speed of stirring is 100rpm per minute-2000rpm per minute; reserving residue after centrifugation; and washing and drying the residue so as to obtain the silicon oxide nano-particles. The reaction speed of the preparation method for the silicon oxide nano-particles is ten or even thousand times that of a conventional method, the phenomenon of particle convergence is reduced, the particles are limited to grow, and the granularity is easy to control and is uniform.
Description
Technical field
The present invention relates to the Synthesis and applications technical field of nano structural material, particularly relate to a kind of preparation method of monox nanometer particle.
Background technology
The development of high-purity, nm-class, production and application and development are important component parts of modern high-tech field.Along with the development of modern science and technology, high-purity, nm-class has been the important source material in the fields such as glass manufacture, silica glass, support of the catalyst, photoconductive fiber, electronics glue, baseplate material.Along with the performance requriements of industrial development to nano silicon oxide powder material is also more and more higher, this just makes the preparation research of nano silicon oxide and application and development be subject to paying close attention to more and more widely.Prepare in the method for nano silica powder, mainly contain chemical Vapor deposition process, elemental silicon combustion method, elemental silicon aqueous-phase oxidation method, the precipitator method, sol-gel method etc.All there is certain defect in these methods: vapor phase process produces nano silicon oxide, and purity is high, and granularity is tiny, but too high to reactor design technical requirements, makes its production cost expensive; Elemental silicon combustion method and elemental silicon aqueous-phase oxidation method can produce the silicon oxide of high-quality, but adopt elemental silicon powder as raw material, and production cost remains high; The monox nanometer grain graininess that other method obtains is wayward, and homogeneity is poor, purity difference, production cycle are long, and all has special requirement to the preparation of product and last handling process, makes it apply and is restricted with expanding production.
Concerning monox nanometer particle, no matter be preparation or application, the dispersion of nano particle is all crucial.Because no matter have employed physics or chemical process prepares nano material, its collection is usually carried out in the solution, and nano particle is easy to reunite under the effect of Van der Waals force.Therefore, how effectively to prevent the reunion of nanoparticle in preparation, drying, accumulating and application process, keep nano-scale, play nanometer effect and advantage, have great theory significance and actual application value to the research of monox nanometer particle.
Summary of the invention
Based on this, be necessary to provide that a kind of granularity is easy to control, the preparation method of the monox nanometer particle of good uniformity.
A preparation method for monox nanometer particle, comprises the steps:
Step one, with organic solvent preparation organoalkoxysilane organic solution, wherein, the carbonatoms of the main chain of described organoalkoxysilane is no more than 5;
Step 2, in the organic solution of described organoalkoxysilane, add acid be placed in microwave chemical reactor, the organic solution that 2min ~ 30min obtains acid organoalkoxysilane is reacted under temperature is 30 DEG C ~ 180 DEG C and mixing speed is the condition of 100rpm/min ~ 2000rpm/min, wherein, the mass ratio of described acid and described organoalkoxysilane is 0.01 ~ 0.1:1, and the microwave frequency range of described microwave chemical reactor is 300MHz ~ 300KMHz;
Step 3, in the organic solution of described acid organoalkoxysilane, add coating materials be placed in described microwave chemical reactor, 2min ~ 30min is reacted under temperature is 30 DEG C ~ 180 DEG C and mixing speed is the condition of 100rpm/min ~ 2000rpm/min, centrifugal rear reservation filter residue, described monox nanometer particle will be obtained after described residue washing, drying, wherein, the mass ratio of described coating materials and described organoalkoxysilane is 0.05 ~ 0.2:1, and the microwave frequency range of described microwave chemical reactor is 300MHz ~ 300KMHz.
In one embodiment, in step one, described organic solvent is acetone, butanone, methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, ethylene glycol or glycerol.
In one embodiment, in step one, in the organic solution of described organoalkoxysilane, the mass percent of organoalkoxysilane is 10% ~ 40%.
In one embodiment, in step one, described organoalkoxysilane is tetramethoxy-silicane, butyl trimethoxy silane, tetraethoxysilane, amyl triethoxysilane, tetrapropoxysilane, Union carbide A-162 or ethyl triethoxysilane.
In one embodiment, in step 2, described microwave chemical reactor is equipped with digital display magnetic stirring apparatus, and power is 1400W.
In one embodiment, in step 2, described acid is hydrochloric acid, nitric acid or sulfuric acid.
In one embodiment, in step 3, the organic acid of described coating materials to be molecular formula be RCOOH or containing silane coupling agent a kind of in double bond, epoxy group(ing), sulfydryl and amido, wherein the carbonatoms of the main chain of R is 6 ~ 20.
In one embodiment, described coating materials is oleic acid, aminopropyl triethoxysilane, γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane, sad or γ-methacryloxypropyl trimethoxy silane.
In one embodiment, in step 3, described coating materials adopts the form of finishing agent solution to add, the solvent of described finishing agent solution is methyl alcohol, ethanol, n-propyl alcohol, Virahol, butanols and isopropylcarbinol, and in described finishing agent solution, the mass percent of coating materials is 1% ~ 10%.
In one embodiment, in step 3, the described centrifugal vacuum that is operating as detaches, by described residue washing be operating as successively with deionized water and alcohol liquid washing and in triplicate, described drying be operating as vacuum-drying 1h ~ 24h at 25 DEG C ~ 100 DEG C.
Preparation method's speed of response of this monox nanometer particle is fast, will accelerate tens of even thousands of times, can reduce the reunion of particle than ordinary method, and the growth of restriction particle, granularity is easy to control, good uniformity.
Accompanying drawing explanation
Fig. 1 is the schema of the preparation method of the monox nanometer particle of an embodiment;
Fig. 2 is the Electronic Speculum figure of monox nanometer particle prepared by embodiment 1;
Fig. 3 is the Electronic Speculum figure of monox nanometer particle prepared by embodiment 2;
Fig. 4 is the Electronic Speculum figure of monox nanometer particle prepared by embodiment 3;
Fig. 5 is the Electronic Speculum figure of monox nanometer particle prepared by embodiment 4;
Fig. 6 is the Electronic Speculum figure of monox nanometer particle prepared by embodiment 5.
Embodiment
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, are described in detail the specific embodiment of the present invention below in conjunction with accompanying drawing.Set forth a lot of detail in the following description so that fully understand the present invention.But the present invention can be much different from alternate manner described here to implement, those skilled in the art can when without prejudice to doing similar improvement when intension of the present invention, therefore the present invention is by the restriction of following public concrete enforcement.
The preparation method of a kind of monox nanometer particle of an embodiment as shown in Figure 1, comprises the steps:
S10, with organic solvent preparation organoalkoxysilane organic solution.
Organic solvent can be acetone, butanone, methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, ethylene glycol or glycerol.
In the organic solution of organoalkoxysilane, the mass percent of organoalkoxysilane is 10% ~ 40%.
The carbonatoms of the main chain of organoalkoxysilane is no more than 5.Concrete, organoalkoxysilane can be tetramethoxy-silicane, butyl trimethoxy silane, tetraethoxysilane, amyl triethoxysilane, tetrapropoxysilane, Union carbide A-162 or ethyl triethoxysilane.
Adding acid in S20, the organic solution of organoalkoxysilane that obtains to S10 is placed in microwave chemical reactor, under temperature is 30 DEG C ~ 180 DEG C and mixing speed is the condition of 100rpm/min ~ 2000rpm/min, react the organic solution that 2min ~ 30min obtains acid organoalkoxysilane.
Acid can be hydrochloric acid, nitric acid or sulfuric acid.
In S20, acid is 0.01 ~ 0.1:1 with the mass ratio of organoalkoxysilane.
Microwave chemical reactor can be equipped with digital display magnetic stirring apparatus, and power is 1400W.The microwave frequency range of microwave chemical reactor can be 300MHz ~ 300KMHz.
Adding coating materials in S30, the organic solution of acid organoalkoxysilane that obtains to S20 is placed in microwave chemical reactor, 2min ~ 30min is reacted under temperature is 30 DEG C ~ 250 DEG C and mixing speed is the condition of 100rpm/min ~ 2000rpm/min, centrifugal rear reservation filter residue, obtains monox nanometer particle by after residue washing, drying.
Microwave chemical reactor can be equipped with digital display magnetic stirring apparatus, and power is 1400W.The microwave frequency range of microwave chemical reactor can be 300MHz ~ 300KMHz.
The microwave frequency range of described microwave chemical reactor is 300MHz ~ 300KMHz.
In S30, the mass ratio of coating materials and organoalkoxysilane is 0.05 ~ 0.2:1.
The organic acid of coating materials to be molecular formula be RCOOH or containing silane coupling agent a kind of in double bond, epoxy group(ing), sulfydryl and amido, wherein the carbonatoms of the main chain of R is 6 ~ 20.Concrete, coating materials can be oleic acid, aminopropyl triethoxysilane, γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane, sad or γ-methacryloxypropyl trimethoxy silane.
In S30, coating materials can adopt the form of finishing agent solution to add, the solvent of finishing agent solution is methyl alcohol, ethanol, n-propyl alcohol, Virahol, butanols and isopropylcarbinol, and in finishing agent solution, the mass percent of coating materials is 1% ~ 10%.
In present embodiment, the centrifugal vacuum that is operating as detaches, and being operating as of residue washing washed also in triplicate with deionized water and alcohol liquid successively, that states drying is operating as vacuum-drying at 25 DEG C ~ 100 DEG C.
Alcohol liquid can be methyl alcohol or ethanol.
Preparation method's speed of response of this monox nanometer particle is fast, will accelerate tens of even thousands of times, can reduce the reunion of particle than ordinary method, and the growth of restriction particle, granularity is easy to control, good uniformity.
Be below specific embodiment, in embodiment 1 ~ 5, microwave chemical reactor is all equipped with digital display magnetic stirring apparatus.
Embodiment 1
Get the tetramethoxy-silicane of 10 grams, be added in 100 grams of methyl alcohol, stir until tetramethoxy-silicane all dissolves, obtain the methanol solution of tetramethoxy-silicane.
In the methanol solution of tetramethoxy-silicane, add 1g hydrochloric acid is placed in microwave chemical reactor, reacts 10min, obtain the methanol solution of acid tetramethoxy-silicane under temperature is 30 DEG C and mixing speed is the condition of 100rpm/min.
Adding 0.5g oleic acid in the methanol solution of oxytropism tetramethoxy-silicane is placed in microwave chemical reactor, 15min is reacted under temperature is 50 DEG C and mixing speed is the condition of 200rpm/min, the microwave frequency of microwave chemical reactor is 200KMHz, vacuum detaches rear reservation filter residue, by filter residue with using deionized water and methanol wash successively also in triplicate, finally at 40 DEG C, vacuum-drying 4h obtains monox nanometer particle.
As shown in Figure 2, as seen from Figure 2, embodiment 1 prepares the epigranular of monox nanometer particle to the Electronic Speculum figure of monox nanometer particle prepared by embodiment 1, particle diameter is about 8nm.
Embodiment 2
Get the tetraethoxysilane of 20 grams, be added in 100 grams of ethanol, stir until tetraethoxysilane all dissolves, obtain the ethanolic soln of tetraethoxysilane.
In the ethanolic soln of tetraethoxysilane, add 2g sulfuric acid is placed in microwave chemical reactor, reacts 15min, obtain the ethanolic soln of acid tetraethoxysilane under temperature is 50 DEG C and mixing speed is the condition of 300rpm/min.
Adding 1g aminopropyl triethoxysilane in the ethanolic soln of oxytropism tetraethoxysilane is placed in microwave chemical reactor, 10min is reacted under temperature is 30 DEG C and mixing speed is the condition of 100rpm/min, the microwave frequency of microwave chemical reactor is 100KMHz, vacuum detaches rear reservation filter residue, by filter residue with using deionized water and washing with alcohol successively also in triplicate, finally at 80 DEG C, vacuum-drying 12h obtains monox nanometer particle.
As shown in Figure 3, as seen from Figure 3, embodiment 2 prepares the epigranular of monox nanometer particle to the Electronic Speculum figure of monox nanometer particle prepared by embodiment 2, particle diameter is about 10nm.
Embodiment 3
Get the tetrapropoxysilane of 15 grams, be added in 100 grams of propyl alcohol, stir until tetrapropoxysilane is all dissolved, obtain the propanol solution of tetrapropoxysilane.
In the propanol solution of tetrapropoxysilane, add 1.5g nitric acid is placed in microwave chemical reactor, reacts 2min, obtain the propanol solution of acid tetrapropoxysilane under temperature is 30 DEG C and mixing speed is the condition of 600rpm/min.
0.5g γ-(2 are added in the propanol solution of oxytropism tetrapropoxysilane, 3-epoxy third oxygen) propyl trimethoxy silicane is placed in microwave chemical reactor, 10min is reacted under temperature is 30 DEG C and mixing speed is the condition of 200rpm/min, the microwave frequency of microwave chemical reactor is 60KMHz, vacuum detaches rear reservation filter residue, by filter residue with using deionized water and washing with alcohol successively also in triplicate, finally at 100 DEG C, vacuum-drying 8h obtains monox nanometer particle.
As shown in Figure 4, as seen from Figure 4, embodiment 3 prepares the epigranular of monox nanometer particle to the Electronic Speculum figure of monox nanometer particle prepared by embodiment 3, particle diameter is about 25nm.
Embodiment 4
Get the butyl trimethoxy silane of 30 grams, be added in 100 grams of acetone, stir until butyl trimethoxy silane all dissolves, obtain the acetone soln of butyl trimethoxy silane.
In the acetone soln of butyl trimethoxy silane, add 1.5g hydrochloric acid is placed in microwave chemical reactor, reacts 25min, obtain the acetone soln of acid butyl trimethoxy silane under temperature is 60 DEG C and mixing speed is the condition of 500rpm/min.
Add in the acetone soln of oxytropism butyl trimethoxy silane that 1g is sad to be placed in microwave chemical reactor, 50min is reacted under temperature is 40 DEG C and mixing speed is the condition of 300rpm/min, the microwave frequency of microwave chemical reactor is 10KMHz, vacuum detaches rear reservation filter residue, by filter residue with using deionized water and washing with alcohol successively also in triplicate, finally at 70 DEG C, vacuum-drying 10h obtains monox nanometer particle.
As shown in Figure 5, as seen from Figure 5, embodiment 4 prepares the epigranular of monox nanometer particle to the Electronic Speculum figure of monox nanometer particle prepared by embodiment 4, particle diameter is about 50nm.
Embodiment 5
Get the tetraethoxysilane of 40 grams, be added in 100 grams of ethanol, stir until tetraethoxysilane all dissolves, obtain the ethanolic soln of tetraethoxysilane.
In the ethanolic soln of tetraethoxysilane, add 1.5g hydrochloric acid is placed in microwave chemical reactor, reacts 5min, obtain the ethanolic soln of acid tetraethoxysilane under temperature is 70 DEG C and mixing speed is the condition of 600rpm/min.
Adding 1.5g γ-methacryloxypropyl trimethoxy silane in the ethanolic soln of oxytropism tetraethoxysilane is placed in microwave chemical reactor, 40min is reacted under temperature is 40 DEG C and mixing speed is the condition of 100rpm/min, the microwave frequency of microwave chemical reactor is 500MHz, vacuum detaches rear reservation filter residue, by filter residue with using deionized water and washing with alcohol successively also in triplicate, finally at 80 DEG C, vacuum-drying 18h obtains monox nanometer particle.
As shown in Figure 6, as seen from Figure 6, embodiment 5 prepares the epigranular of monox nanometer particle to the Electronic Speculum figure of monox nanometer particle prepared by embodiment 5, particle diameter is about 100nm.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (9)
1. a preparation method for monox nanometer particle, is characterized in that, comprises the steps:
Step one, with organic solvent preparation organoalkoxysilane organic solution, wherein, the carbonatoms of the main chain of described organoalkoxysilane is no more than 5;
Step 2, in the organic solution of described organoalkoxysilane, add acid be placed in microwave chemical reactor, the organic solution that 2min ~ 30min obtains acid organoalkoxysilane is reacted under temperature is 30 DEG C ~ 180 DEG C and mixing speed is the condition of 100rpm/min ~ 2000rpm/min, wherein, the mass ratio of described acid and described organoalkoxysilane is 0.01 ~ 0.1:1, and the microwave frequency range of described microwave chemical reactor is 300MHz ~ 300KMHz;
Step 3, in the organic solution of described acid organoalkoxysilane, add coating materials be placed in described microwave chemical reactor, 2min ~ 30min is reacted under temperature is 30 DEG C ~ 180 DEG C and mixing speed is the condition of 100rpm/min ~ 2000rpm/min, centrifugal rear reservation filter residue, described monox nanometer particle will be obtained after described residue washing, drying, wherein, the mass ratio of described coating materials and described organoalkoxysilane is 0.05 ~ 0.2:1, and the microwave frequency range of described microwave chemical reactor is 300MHz ~ 300KMHz;
The organic acid of described coating materials to be molecular formula be RCOOH, wherein the carbonatoms of the main chain of R is 6 ~ 20.
2. the preparation method of monox nanometer particle according to claim 1, is characterized in that, in step one, described organic solvent is acetone, butanone, methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, ethylene glycol or glycerol.
3. the preparation method of monox nanometer particle according to claim 1, is characterized in that, in step one, in the organic solution of described organoalkoxysilane, the mass percent of organoalkoxysilane is 10% ~ 40%.
4. the preparation method of monox nanometer particle according to claim 1, it is characterized in that, in step one, described organoalkoxysilane is tetramethoxy-silicane, butyl trimethoxy silane, tetraethoxysilane, amyl triethoxysilane, tetrapropoxysilane, Union carbide A-162 or ethyl triethoxysilane.
5. the preparation method of monox nanometer particle according to claim 1, is characterized in that, in step 2, described microwave chemical reactor is equipped with digital display magnetic stirring apparatus, and power is 1400W.
6. the preparation method of monox nanometer particle according to claim 1, is characterized in that, in step 2, described acid is hydrochloric acid, nitric acid or sulfuric acid.
7. the preparation method of monox nanometer particle according to claim 1, is characterized in that, described coating materials is oleic acid or sad.
8. the preparation method of monox nanometer particle according to claim 1, it is characterized in that, in step 3, described coating materials adopts the form of finishing agent solution to add, the solvent of described finishing agent solution is methyl alcohol, ethanol, n-propyl alcohol, Virahol, butanols and isopropylcarbinol, and in described finishing agent solution, the mass percent of coating materials is 1% ~ 10%.
9. the preparation method of monox nanometer particle according to claim 1, it is characterized in that, in step 3, the described centrifugal vacuum that is operating as detaches, by described residue washing be operating as successively with deionized water and alcohol liquid washing and in triplicate, described drying be operating as vacuum-drying 1h ~ 24h at 25 DEG C ~ 100 DEG C.
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| CN1557778A (en) * | 2004-02-03 | 2004-12-29 | 同济大学 | Process for preparation of nano multiporous silicon dioxide aerogel block |
| CN1657410A (en) * | 2005-01-20 | 2005-08-24 | 辽宁大学 | Method for modifying surface of manometer |
| CN101117221A (en) * | 2007-07-19 | 2008-02-06 | 东华大学 | Method for preparing monodisperse magnetic silica dioxide nano particles |
| CN101633505A (en) * | 2009-08-25 | 2010-01-27 | 郑文芝 | SiO2 nanoscale porous material with aerogel property prepared by microwave reaction and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1557778A (en) * | 2004-02-03 | 2004-12-29 | 同济大学 | Process for preparation of nano multiporous silicon dioxide aerogel block |
| CN1657410A (en) * | 2005-01-20 | 2005-08-24 | 辽宁大学 | Method for modifying surface of manometer |
| CN101117221A (en) * | 2007-07-19 | 2008-02-06 | 东华大学 | Method for preparing monodisperse magnetic silica dioxide nano particles |
| CN101633505A (en) * | 2009-08-25 | 2010-01-27 | 郑文芝 | SiO2 nanoscale porous material with aerogel property prepared by microwave reaction and preparation method thereof |
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Effective date of registration: 20230703 Address after: 518103 Longwangmiao Industrial Zone, Fuyong street, Bao'an District, Shenzhen City, Guangdong Province Patentee after: Shenzhen advanced electronic materials International Innovation Research Institute Address before: 1068 No. 518055 Guangdong city in Shenzhen Province, Nanshan District City Xili University School Avenue Patentee before: SHENZHEN INSTITUTES OF ADVANCED TECHNOLOGY CHINESE ACADEMY OF SCIENCES |