CN1244492C - Synthesis method of monodispersed nano-mesopore silicon dioxide material - Google Patents
Synthesis method of monodispersed nano-mesopore silicon dioxide material Download PDFInfo
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- CN1244492C CN1244492C CN 200310105133 CN200310105133A CN1244492C CN 1244492 C CN1244492 C CN 1244492C CN 200310105133 CN200310105133 CN 200310105133 CN 200310105133 A CN200310105133 A CN 200310105133A CN 1244492 C CN1244492 C CN 1244492C
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 239000000463 material Substances 0.000 title claims abstract description 31
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 28
- 235000012239 silicon dioxide Nutrition 0.000 title abstract description 7
- 238000001308 synthesis method Methods 0.000 title 1
- 239000004094 surface-active agent Substances 0.000 claims abstract description 12
- 238000010189 synthetic method Methods 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000003513 alkali Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 239000013543 active substance Substances 0.000 claims description 11
- 241000282326 Felis catus Species 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 8
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- 229920000570 polyether Polymers 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 239000003637 basic solution Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- 239000004743 Polypropylene Substances 0.000 claims description 3
- XJWSAJYUBXQQDR-UHFFFAOYSA-M dodecyltrimethylammonium bromide Chemical group [Br-].CCCCCCCCCCCC[N+](C)(C)C XJWSAJYUBXQQDR-UHFFFAOYSA-M 0.000 claims description 3
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000004115 Sodium Silicate Substances 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 2
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 2
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- XXZNHVPIQYYRCG-UHFFFAOYSA-N trihydroxy(propoxy)silane Chemical compound CCCO[Si](O)(O)O XXZNHVPIQYYRCG-UHFFFAOYSA-N 0.000 claims description 2
- SZEMGTQCPRNXEG-UHFFFAOYSA-M trimethyl(octadecyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C SZEMGTQCPRNXEG-UHFFFAOYSA-M 0.000 claims description 2
- 229960004418 trolamine Drugs 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000011148 porous material Substances 0.000 abstract description 13
- 239000003082 abrasive agent Substances 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 239000002114 nanocomposite Substances 0.000 abstract description 3
- 230000003287 optical effect Effects 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000012295 chemical reaction liquid Substances 0.000 abstract 2
- 125000002091 cationic group Chemical group 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 229920002521 macromolecule Polymers 0.000 abstract 1
- 238000005498 polishing Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000012798 spherical particle Substances 0.000 abstract 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 24
- 239000002245 particle Substances 0.000 description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 18
- 230000005540 biological transmission Effects 0.000 description 13
- 229910021529 ammonia Inorganic materials 0.000 description 12
- 238000002441 X-ray diffraction Methods 0.000 description 9
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- 238000002336 sorption--desorption measurement Methods 0.000 description 9
- 238000000018 DNA microarray Methods 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 102220500397 Neutral and basic amino acid transport protein rBAT_M41T_mutation Human genes 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 239000013335 mesoporous material Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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Abstract
The present invention relates to a synthetic method of a monodisperse nano mesoporous silicon dioxide, which belongs to the technical field of inorganic nano materials. In the method, a collosol reaction liquid is formed from a cationic surface active agent as a template agent, and a triblock nonionic surface active agent as an auxiliary template agent and a dispersing agent under the mild alkali conditions, and the collosol reaction liquid is synthesized into the monodisperse nano mesoporous silicon dioxide material. The mesoporous silicon dioxide material synthesized with the method has the advantages of uniform nano level monodisperse spherical particle, better ordered mesoporous pore canal, superior specific surface area and larger pore volume, and thus, the mesoporous silicon dioxide material has wide application prospects on the aspects of catalysis, macromolecule separation, sensors, optical materials, biological chips, organic-inorganic nano composite materials, chemico-mechanical polishing abrasive materials, etc.
Description
Technical field
The invention belongs to technical field of inorganic nanometer material, be specifically related to a kind of synthetic method of monodisperse nanosized mesoporous silica material.
Technical background
U.S. Mobil company released M41S series mesopore molecular sieve first in 1992.This class material has broad application prospects at aspects such as catalysis, fractionation by adsorption, transmitter, optical material, biochip, organic-inorganic nanocomposite and chemically machinery polished abrasive materials.Wherein MCM-41 is owing to have uniform six sides arrangement mesopore orbit, higher specific surface area, plurality of advantages such as thermostability and potential catalytic performance and receive the concern of Chinese scholars preferably always.At present people have obtained remarkable progress at MCM-41 aspect preparing, and have synthesized hexagonal mesoporous film, block, fiber, micropowder and nano powder etc. in succession.Nano level MCM-41 powder has dual nanostructure, i.e. nano-scale particle sizes and nano level meso-hole structure, be expected to be applied in a lot of key areas, but as other nano-powder, very easily reunite because of its special surface tissue, the existence of coacervate has a strong impact on its performance and application.But the at present domestic relevant research that solves mesoporous nano silicon dioxide powder reuniting problem also is a blank, and this has limited its application greatly.
Summary of the invention
The synthetic method that the purpose of this invention is to provide a kind of monodisperse nanosized mesoporous silica material, this method uses three block nonionogenic tensides to gather oxyethylene-poly-propylene oxide-poly-oxyethylene (PEO-PPO-PEO) as auxiliary template agent and dispersion agent, form colloidal sol shape reaction solution, and then synthesize single dispersion, the even spherical monodisperse nanosized mesoporous silica material of order nano level good, that specific surface area is high.
Technical scheme of the present invention is:
A kind of synthetic method of monodisperse nanosized mesoporous silica material under gentle alkaline condition, is a template with the cats product, is auxiliary template agent and dispersion agent with three block polyether nonionogenic tensides, and concrete synthesis step is as follows:
1) cats product and three block polyether nonionogenic tensides are joined in the basic solution, fully stir down at 30～80 ℃, after treating that tensio-active agent dissolves fully, the silicon source is joined in this solution, the mol ratio in deionized water, alkali source, cats product, three block polyether nonionogenic tensides and silicon source is respectively: 60～2000,0.20～100.0,0.05～0.50,0.001～0.40, continuously stirring is 0.25～4.0 hour under 20-70 ℃ of temperature of reaction, generates collosol intermixture;
2) collosol intermixture that step 1 is obtained is transferred in the thermostatic drying chamber, at 60～150 ℃ of oven dry moisture, obtains the white powder product;
3) product with step 2 after 6～10 hours, promptly obtains the monodisperse nanosized mesoporous silica material of white powder through 500 ℃～600 ℃ high-temperature roastings.
Three block polyether nonionogenic tensides of the present invention are poly-oxyethylene-poly-propylene oxide-poly-oxyethylene (PEO-PPO-PEO) tensio-active agent, and molecular weight is 2000～100000.
Cats product of the present invention is that carbon chain lengths is C
8-C
22Long chain quaternary.
Cats product of the present invention, it is a kind of of long-chain quaternary ammonium salts such as Trimethyllaurylammonium bromide, cetyl trimethylammonium bromide, octadecyl trimethylammonium bromide.
Silicon of the present invention source is a kind of of tetraethoxy, methyl silicate, positive silicic acid propyl ester, sodium metasilicate, silicon sol, water glass and white carbon black.
Basic solution of the present invention is the aqueous solution a kind of of sodium hydroxide, potassium hydroxide, ammoniacal liquor, Monoethanolamine MEA BASF, diethanolamine, trolamine.
Step 3) high-temperature calcination process of the present invention heats up with 1～5 ℃/min speed.
Advantage of the present invention and beneficial effect are:
The synthetic method of the monodisperse nanosized mesoporous silica MCM-41 material that the present invention proposes, with the cats product is template, three block nonionogenic tensides are auxiliary template agent and dispersion agent, under gentle alkaline condition, form the colloidal sol reaction solution, and then synthesize the monodisperse nanosized mesoporous silica material, the gained Metaporous silicon dioxide material is two-dimentional hexagonal structure MCM-41, this method synthetic Metaporous silicon dioxide material has the nano level spheroidal particle that singly is uniformly dispersed, has ordered mesoporous pore canals preferably, have higher specific surface area and bigger pore volume, it is even sphere, monodispersed, but particle diameter modulation in 50～120nm scope, order is good, specific surface area is high, catalysis can be satisfied at the mesoporous material of 3～6nm in the aperture, macromole separates, transmitter, optical material, biochip, many-sided demand in fields such as organic-inorganic nanocomposite and chemically machinery polished abrasive material.
Description of drawings
Fig. 1 (a) is the particle transmission electron microscope photo of embodiment 3.
Fig. 1 (b) is the particle transmission electron microscope photo of embodiment 1.
Fig. 1 (c) is the particle transmission electron microscope photo of embodiment 6.
Fig. 2 is the XRD spectra of the sample of embodiment 7.
Fig. 3 (a) is the nitrogen adsorption desorption curve of embodiment 1.
Fig. 3 (b) is the pore distribution curve of embodiment 1.
Embodiment
The invention will be further described below by embodiment.
Embodiment 1
With 6.0g cetyl trimethylammonium bromide and 10.56g F127 (PEO-PPO-PEO, molecular-weight average 11000), is dissolved in (ammonia vol 36.96g) in the 600g ammonia soln, fully stirs down at 35 ℃, after treating that tensio-active agent dissolves fully, add the 20g tetraethoxy, at room temperature continuously stirring is 2 hours, obtains vitreosol, be transferred in the thermostatic drying chamber, 100 ℃ of oven dry moisture obtain white powder, and 550 ℃ of high-temperature roastings 6 hours obtain final monodisperse nanosized mesoporous silica material.
Fig. 1 (b) is the particle transmission electron microscope photo of sample, transmission electron microscope photo is shown as monodispersed even spheroidal particle, particle diameter is 70～80nm, XRD spectra is shown as orderly hexagonal mesoporous structure, Fig. 3 (a) and Fig. 3 (b) are nitrogen adsorption desorption curve and the pore distribution curve of embodiment 1, nitrogen adsorption desorption spectrogram is shown as the meso-hole structure of pore size distribution homogeneous, and specific surface area is 800m
2About/g, the aperture is 4-5nm.
With 5.2g Trimethyllaurylammonium bromide and 10.56g F127 (PEO-PPO-PEO, molecular-weight average 11000), is dissolved in (ammonia vol 61.60g) in the 600g ammonia soln, fully stirs down at 30 ℃, after treating that tensio-active agent dissolves fully, add tetraethoxy 20g,, obtain vitreosol 30 ℃ of following continuously stirring 4 hours, be transferred in the thermostatic drying chamber, 80 ℃ of oven dry moisture obtain white powder, and 550 ℃ of high-temperature roastings 6 hours obtain final monodisperse nanosized mesoporous silica material.
Transmission electron microscope photo is shown as monodispersed even spheroidal particle, and particle diameter is about 100nm, and XRD spectra is shown as orderly hexagonal mesoporous structure, and nitrogen adsorption desorption spectrogram is shown as the meso-hole structure of pore size distribution homogeneous, and specific surface area is 900m
2About/g, the aperture is 2-3nm.
Embodiment 3
With 6.0g cetyl trimethylammonium bromide and 5.28g F127 (PEO-PPO-PEO, molecular-weight average 11000), be dissolved in (2M sodium hydroxide 14.5ml) in the 1500g sodium hydroxide solution, fully stir down at 80 ℃, after treating that tensio-active agent dissolves fully, add tetraethoxy 20g, 40 ℃ of following continuously stirring 1 hour, obtain vitreosol, be transferred in the thermostatic drying chamber, 80 ℃ of oven dry moisture obtain white powder, and 550 ℃ of high-temperature roastings 10 hours obtain final monodisperse nanosized mesoporous silica material.
Fig. 1 (a) is the particle transmission electron microscope photo, transmission electron microscope photo is shown as monodispersed even spheroidal particle, and particle diameter is 50～60nm, and XRD spectra is shown as orderly hexagonal mesoporous structure, nitrogen adsorption desorption spectrogram is shown as the meso-hole structure of pore size distribution homogeneous, and specific surface area is 800m
2About/g, the aperture is 4～5nm.
Embodiment 4
With 6.0g cetyl trimethylammonium bromide and 5.28g F127 (PEO-PPO-PEO, molecular-weight average 11000), is dissolved in (ammonia vol 36.96g) in the 600g ammonia soln, fully stirs down at 40 ℃, after treating that tensio-active agent dissolves fully, add methyl silicate 15g, at room temperature continuously stirring is 2 hours, obtains vitreosol, be transferred in the thermostatic drying chamber, 80 ℃ of oven dry moisture obtain white powder, and 550 ℃ of high-temperature roastings 6 hours obtain final monodisperse nanosized mesoporous silica material.
Transmission electron microscope photo is shown as monodispersed even spheroidal particle, and particle diameter is 80～90nm, and XRD spectra is shown as orderly hexagonal mesoporous structure, and nitrogen adsorption desorption spectrogram is shown as the meso-hole structure of pore size distribution homogeneous, and specific surface area is 700m
2About/g, the aperture is 4～5nm.
Embodiment 5
With 4.0g cetyl trimethylammonium bromide and 12.24g F68 (PEO-PPO-PEO, molecular-weight average 8500), is dissolved in (ammonia vol 36.96g) in the 1000g ammonia soln, fully stirs down at 70 ℃, after treating that tensio-active agent dissolves fully, add tetraethoxy 20g, at room temperature continuously stirring is 2 hours, obtains vitreosol, be transferred in the thermostatic drying chamber, 80 ℃ of oven dry moisture obtain white powder, and 550 ℃ of high-temperature roastings 6 hours obtain final monodisperse nanosized mesoporous silica material.
Transmission electron microscope photo is shown as monodispersed even spheroidal particle, and particle diameter is 70～80nm, and XRD spectra is shown as orderly hexagonal mesoporous structure, and nitrogen adsorption desorption spectrogram is shown as the meso-hole structure of pore size distribution homogeneous, and specific surface area is 700m
2About/g, the aperture is 5～6nm.
Embodiment 6
With 4.0g cetyl trimethylammonium bromide and 12.24g F68 (PEO-PPO-PEO, molecular-weight average 8500), is dissolved in (ammonia vol 73.92g) in the 300g ammonia soln, fully stirs down at 50 ℃, after treating that tensio-active agent dissolves fully, add tetraethoxy 20g, at room temperature continuously stirring is 4 hours, obtains vitreosol, be transferred in the thermostatic drying chamber, 80 ℃ of oven dry moisture obtain white powder, and 600 ℃ of high-temperature roastings 10 hours obtain final monodisperse nanosized mesoporous silica material.
Particle transmission electron microscope photo shown in Fig. 1 (c), transmission electron microscope photo is shown as monodispersed even spheroidal particle, and particle diameter is 100～120nm, and XRD spectra is shown as orderly hexagonal mesoporous structure, nitrogen adsorption desorption spectrogram is shown as the meso-hole structure of pore size distribution homogeneous, and specific surface area is 700m
2About/g, the aperture is 5～6nm.
Embodiment 7
With 4.0g cetyl trimethylammonium bromide and 12.24g F68 (PEO-PPO-PEO, molecular-weight average 8500), is dissolved in (ammonia vol 36.96g) in the 800g ammonia soln, fully stirs down at 60 ℃, after treating that tensio-active agent dissolves fully, add tetraethoxy 20g,, obtain vitreosol 60 ℃ of following continuously stirring 20 minutes, be transferred in the thermostatic drying chamber, 80 ℃ of oven dry moisture obtain white powder, and 550 ℃ of high-temperature roastings 6 hours obtain final monodisperse nanosized mesoporous silica material.
Transmission electron microscope photo is shown as monodispersed even spheroidal particle, particle diameter is 70～80nm, the XRD spectra of sample as shown in Figure 2, and XRD spectra is shown as orderly hexagonal mesoporous structure, nitrogen adsorption desorption spectrogram is shown as the meso-hole structure of pore size distribution homogeneous, and specific surface area is 700m
2About/g, the aperture is 4～5nm.
Claims (5)
1, a kind of synthetic method of monodisperse nanosized mesoporous silica material, it is characterized in that: under alkaline condition, with the cats product is template, is auxiliary template agent and dispersion agent with three block polyether nonionogenic tensides, and concrete synthesis step is as follows:
1) cats product and three block polyether nonionogenic tensides are joined in the basic solution, fully stir down at 30～80 ℃, after treating that tensio-active agent dissolves fully, the silicon source is joined in this solution, the mol ratio in deionized water, alkali source, cats product, three block polyether nonionogenic tensides and silicon source is respectively: 60～2000,0.20～100.0,0.05～0.50,0.001～0.40, continuously stirring is 0.25～4.0 hour under 20-70 ℃ of temperature of reaction, generates collosol intermixture;
2) collosol intermixture that step 1 is obtained is transferred in the thermostatic drying chamber, at 60～150 ℃ of oven dry moisture, obtains the white powder product;
3) product with step 2 after 6～10 hours, promptly obtains the monodisperse nanosized mesoporous silica material of white powder through 500 ℃～600 ℃ high-temperature roastings;
Described three block polyether nonionogenic tensides are poly-oxyethylene-poly-propylene oxide-poly-oxyethylene tensio-active agent, and molecular weight is 2000～100000; Described cats product is that carbon chain lengths is the long chain quaternary of C8-C22.
2, the synthetic method of monodisperse nanosized mesoporous silica material according to claim 1 is characterized in that: described long chain quaternary is Trimethyllaurylammonium bromide, cetyl trimethylammonium bromide or octadecyl trimethylammonium bromide.
3, the synthetic method of monodisperse nanosized mesoporous silica material according to claim 1 is characterized in that: described silicon source is a kind of of tetraethoxy, methyl silicate, positive silicic acid propyl ester, sodium metasilicate, silicon sol, water glass and white carbon black.
4, the synthetic method of monodisperse nanosized mesoporous silica according to claim 1 is characterized in that: described basic solution is the aqueous solution a kind of of sodium hydroxide, potassium hydroxide, ammoniacal liquor, Monoethanolamine MEA BASF, diethanolamine, trolamine.
5, the synthetic method of monodisperse nanosized mesoporous silica according to claim 1 is characterized in that: described step 3) high-temperature calcination process heats up with 1～5 ℃/min speed.
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|---|---|---|---|---|
| US9818498B2 (en) | 2011-10-25 | 2017-11-14 | Lg Innotek Co., Ltd. | Paste composition for printing and touch panel |
| CN103087676A (en) * | 2013-01-29 | 2013-05-08 | 淄博理研泰山涂附磨具有限公司 | Sintering method of abrasion resisting abrasive particles |
| CN103087676B (en) * | 2013-01-29 | 2014-07-30 | 淄博理研泰山涂附磨具有限公司 | Sintering method of abrasion resisting abrasive particles |
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