CN103172076A - Preparation method for silicon oxide nano-particles - Google Patents
Preparation method for silicon oxide nano-particles Download PDFInfo
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- CN103172076A CN103172076A CN2013101024314A CN201310102431A CN103172076A CN 103172076 A CN103172076 A CN 103172076A CN 2013101024314 A CN2013101024314 A CN 2013101024314A CN 201310102431 A CN201310102431 A CN 201310102431A CN 103172076 A CN103172076 A CN 103172076A
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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 preparation and the applied technical field of nano structural material, particularly relate to a kind of preparation method of monox nanometer particle.
Background technology
Development, production and application and development high-purity, nm-class 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 industrial development is also more and more higher to the performance requriements of nano silicon oxide powder material, 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 is produced nano silicon oxide, and purity is high, and granularity is tiny, but too high to the reactor design technical requirements, makes its production cost expensive; Elemental silicon combustion method and elemental silicon aqueous phase oxidation method can be produced high-quality silicon oxide, but adopt the elemental silicon powder as raw material, and production cost is high; The monox nanometer grain graininess that other method obtains is wayward, and homogeneity is relatively poor, purity difference, production cycle are long, and preparation and the last handling process of product all had special requirement, it is used and expanding production is restricted.
Concerning the monox nanometer particle, no matter be preparation or application, the dispersion of nano particle is all crucial.Because no matter adopted physics or chemical process prepares nano material, its collection is usually carried out in solution, 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, dry, accumulating and application process, keep nano-scale, performance 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 kind of preparation method of monox nanometer particle comprises the steps:
Step 1, with the organic solution of organic solvent preparation organoalkoxysilane, wherein, the carbonatoms of the main chain of described organoalkoxysilane is no more than 5;
Step 2, add acid to be placed in microwave chemical reactor in the organic solution of described organoalkoxysilane, be that 30 ℃～180 ℃ and mixing speed are to react the organic solution that 2min～30min obtains acid organoalkoxysilane under the condition of 100rpm/min～2000rpm/min in temperature, 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, add coating materials to be placed in described microwave chemical reactor in the organic solution of described acid organoalkoxysilane, be that 30 ℃～180 ℃ and mixing speed are to react 2min～30min under the condition of 100rpm/min～2000rpm/min in temperature, 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 1, described organic solvent is acetone, butanone, methyl alcohol, ethanol, propyl alcohol, Virahol, butanols, ethylene glycol or glycerol.
In one embodiment, in step 1, in the organic solution of described organoalkoxysilane, the mass percent of organoalkoxysilane is 10%～40%.
In one embodiment, in step 1, 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 the 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, described coating materials is that molecular formula is the organic acid of RCOOH or contains a kind of silane coupling agent in two keys, epoxy group(ing), sulfydryl and amido, and 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 the 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, with being operating as successively with deionized water and the washing of pure liquid and triplicate of described residue washing, and being operating as at 25 ℃～100 ℃ lower vacuum-drying 1h～24h of described drying.
Preparation method's speed of response of this monox nanometer particle is fast, will accelerate tens of even thousands of times than ordinary method, can reduce the reunion of particle, the growth of restriction particle, and granularity is easy to control, good uniformity.
Description of drawings
Fig. 1 is preparation method's the schema of the monox nanometer particle of an embodiment;
Fig. 2 is the Electronic Speculum figure of the monox nanometer particle of embodiment 1 preparation;
Fig. 3 is the Electronic Speculum figure of the monox nanometer particle of embodiment 2 preparations;
Fig. 4 is the Electronic Speculum figure of the monox nanometer particle of embodiment 3 preparations;
Fig. 5 is the Electronic Speculum figure of the monox nanometer particle of embodiment 4 preparations;
Fig. 6 is the Electronic Speculum figure of the monox nanometer particle of embodiment 5 preparations.
Embodiment
For above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.A lot of details have been set forth in the following description so that fully understand the present invention.But the present invention can implement much to be different from alternate manner described here, and those skilled in the art can be in the situation that do similar improvement without prejudice to intension of the present invention, so the present invention is not subjected to 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 the organic solution of organic solvent preparation organoalkoxysilane.
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 to be placed in microwave chemical reactor in the organic solution of S20, the organoalkoxysilane that obtains to S10, is that 30 ℃～180 ℃ and mixing speed are to react the organic solution that 2min～30min obtains acid organoalkoxysilane under the condition of 100rpm/min～2000rpm/min in temperature.
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 the digital display magnetic stirring apparatus, and power is 1400W.The microwave frequency range of microwave chemical reactor can be 300MHz～300KMHz.
Add coating materials to be placed in microwave chemical reactor in the organic solution of S30, the acid organoalkoxysilane that obtains to S20, be that 30 ℃～250 ℃ and mixing speed are to react 2min～30min under the condition of 100rpm/min～2000rpm/min in temperature, centrifugal rear reservation filter residue will obtain the monox nanometer particle after residue washing, drying.
Microwave chemical reactor can be equipped with the 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.
Coating materials is that molecular formula is the organic acid of RCOOH or contains a kind of silane coupling agent in two keys, epoxy group(ing), sulfydryl and amido, and 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 the 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 the 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 successively of residue washing washed and triplicate with deionized water and pure liquid, states dry being operating as 25 ℃～100 ℃ lower vacuum-dryings.
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 than ordinary method, can reduce the reunion of particle, the growth of restriction particle, and granularity is easy to control, good uniformity.
Be below specific embodiment, in embodiment 1～5, microwave chemical reactor all is equipped with the digital display magnetic stirring apparatus.
Embodiment 1
Get the tetramethoxy-silicane of 10 grams, be added in 100 gram methyl alcohol, stir until tetramethoxy-silicane all dissolves, obtain the methanol solution of tetramethoxy-silicane.
Adding 1g hydrochloric acid to be placed in microwave chemical reactor in the methanol solution of tetramethoxy-silicane, is that 30 ℃ and mixing speed are to react 10min under the condition of 100rpm/min in temperature, obtains the methanol solution of acid tetramethoxy-silicane.
Add 0.5g oleic acid to be placed in microwave chemical reactor in the methanol solution of oxytropism tetramethoxy-silicane, be that 50 ℃ and mixing speed are to react 15min under the condition of 200rpm/min in temperature, the microwave frequency of microwave chemical reactor is 200KMHz, vacuum detaches rear reservation filter residue, filter residue with using successively deionized water and methanol wash and triplicate, is obtained the monox nanometer particle at 40 ℃ of lower vacuum-drying 4h at last.
The Electronic Speculum figure of the monox nanometer particle of embodiment 1 preparation as shown in Figure 2, as seen from Figure 2, epigranular, particle diameter that embodiment 1 prepares the monox nanometer particle are about 8nm.
Embodiment 2
Get the tetraethoxysilane of 20 grams, be added in 100 gram ethanol, stir until tetraethoxysilane all dissolves, obtain the ethanolic soln of tetraethoxysilane.
Adding 2g sulfuric acid to be placed in microwave chemical reactor in the ethanolic soln of tetraethoxysilane, is that 50 ℃ and mixing speed are to react 15min under the condition of 300rpm/min in temperature, obtains the ethanolic soln of acid tetraethoxysilane.
Add the 1g aminopropyl triethoxysilane to be placed in microwave chemical reactor in the ethanolic soln of oxytropism tetraethoxysilane, be that 30 ℃ and mixing speed are to react 10min under the condition of 100rpm/min in temperature, the microwave frequency of microwave chemical reactor is 100KMHz, vacuum detaches rear reservation filter residue, filter residue with using successively deionized water and washing with alcohol and triplicate, is obtained the monox nanometer particle at 80 ℃ of lower vacuum-drying 12h at last.
The Electronic Speculum figure of the monox nanometer particle of embodiment 2 preparation as shown in Figure 3, as seen from Figure 3, epigranular, particle diameter that embodiment 2 prepares the monox nanometer particle are about 10nm.
Embodiment 3
Get the tetrapropoxysilane of 15 grams, be added in 100 gram propyl alcohol, stir until tetrapropoxysilane is all dissolved, obtain the propanol solution of tetrapropoxysilane.
Adding 1.5g nitric acid to be placed in microwave chemical reactor in the propanol solution of tetrapropoxysilane, is that 30 ℃ and mixing speed are to react 2min under the condition of 600rpm/min in temperature, obtains the propanol solution of acid tetrapropoxysilane.
Add 0.5g γ-(2 in the propanol solution of oxytropism tetrapropoxysilane, 3-epoxy the third oxygen) propyl trimethoxy silicane is placed in microwave chemical reactor, be that 30 ℃ and mixing speed are to react 10min under the condition of 200rpm/min in temperature, the microwave frequency of microwave chemical reactor is 60KMHz, vacuum detaches rear reservation filter residue, filter residue with using successively deionized water and washing with alcohol and triplicate, is obtained the monox nanometer particle at 100 ℃ of lower vacuum-drying 8h at last.
The Electronic Speculum figure of the monox nanometer particle of embodiment 3 preparation as shown in Figure 4, as seen from Figure 4, epigranular, particle diameter that embodiment 3 prepares the monox nanometer particle are about 25nm.
Embodiment 4
Get the butyl trimethoxy silane of 30 grams, be added in 100 gram acetone, stir until butyl trimethoxy silane all dissolves, obtain the acetone soln of butyl trimethoxy silane.
Adding 1.5g hydrochloric acid to be placed in microwave chemical reactor in the acetone soln of butyl trimethoxy silane, is that 60 ℃ and mixing speed are to react 25min under the condition of 500rpm/min in temperature, obtains the acetone soln of acid butyl trimethoxy silane.
Add in the acetone soln of oxytropism butyl trimethoxy silane that 1g is sad to be placed in microwave chemical reactor, be that 40 ℃ and mixing speed are to react 50min under the condition of 300rpm/min in temperature, the microwave frequency of microwave chemical reactor is 10KMHz, vacuum detaches rear reservation filter residue, filter residue with using successively deionized water and washing with alcohol and triplicate, is obtained the monox nanometer particle at 70 ℃ of lower vacuum-drying 10h at last.
The Electronic Speculum figure of the monox nanometer particle of embodiment 4 preparation as shown in Figure 5, as seen from Figure 5, epigranular, particle diameter that embodiment 4 prepares the monox nanometer particle are about 50nm.
Embodiment 5
Get the tetraethoxysilane of 40 grams, be added in 100 gram ethanol, stir until tetraethoxysilane all dissolves, obtain the ethanolic soln of tetraethoxysilane.
Adding 1.5g hydrochloric acid to be placed in microwave chemical reactor in the ethanolic soln of tetraethoxysilane, is that 70 ℃ and mixing speed are to react 5min under the condition of 600rpm/min in temperature, obtains the ethanolic soln of acid tetraethoxysilane.
Add 1.5g γ-methacryloxypropyl trimethoxy silane to be placed in microwave chemical reactor in the ethanolic soln of oxytropism tetraethoxysilane, be that 40 ℃ and mixing speed are to react 40min under the condition of 100rpm/min in temperature, the microwave frequency of microwave chemical reactor is 500MHz, vacuum detaches rear reservation filter residue, filter residue with using successively deionized water and washing with alcohol and triplicate, is obtained the monox nanometer particle at 80 ℃ of lower vacuum-drying 18h at last.
The Electronic Speculum figure of the monox nanometer particle of embodiment 5 preparation as shown in Figure 6, as seen from Figure 6, epigranular, particle diameter that embodiment 5 prepares the monox nanometer particle are about 100nm.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.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 (10)
1. the preparation method of a monox nanometer particle, is characterized in that, comprises the steps:
Step 1, with the organic solution of organic solvent preparation organoalkoxysilane, wherein, the carbonatoms of the main chain of described organoalkoxysilane is no more than 5;
Step 2, add acid to be placed in microwave chemical reactor in the organic solution of described organoalkoxysilane, be that 30 ℃～180 ℃ and mixing speed are to react the organic solution that 2min～30min obtains acid organoalkoxysilane under the condition of 100rpm/min～2000rpm/min in temperature, 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, add coating materials to be placed in described microwave chemical reactor in the organic solution of described acid organoalkoxysilane, be that 30 ℃～180 ℃ and mixing speed are to react 2min～30min under the condition of 100rpm/min～2000rpm/min in temperature, 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.
2. the preparation method of monox nanometer particle according to claim 1, is characterized in that, in step 1, 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 1, 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 1, 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 the 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, it is characterized in that, in step 3, described coating materials is that molecular formula is the organic acid of RCOOH or contains a kind of silane coupling agent in two keys, epoxy group(ing), sulfydryl and amido, and wherein the carbonatoms of the main chain of R is 6～20.
8. the preparation method of monox nanometer particle according to claim 7, it is characterized in that, described coating materials is oleic acid, aminopropyl triethoxysilane, γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane, sad or γ-methacryloxypropyl trimethoxy silane.
9. 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%.
10. 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, with being operating as successively with deionized water and the washing of pure liquid and triplicate of described residue washing, being operating as at 25 ℃～100 ℃ lower vacuum-drying 1h～24h of described drying.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106596482A (en) * | 2016-12-08 | 2017-04-26 | 哈尔滨师范大学 | Fluorescent silica nanoparticle and application thereof in mercury ion detection and fingerprint development |
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| 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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| 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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| CN106596482A (en) * | 2016-12-08 | 2017-04-26 | 哈尔滨师范大学 | Fluorescent silica nanoparticle and application thereof in mercury ion detection and fingerprint development |
| CN106596482B (en) * | 2016-12-08 | 2019-04-30 | 哈尔滨师范大学 | Fluorescence silicon nano particles and its application in mercury ion detecting and fingerprint manifestation |
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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 |