CN101857234B - Monodisperse mesoporous silicon dioxide hollow nano-microsphere and preparation method - Google Patents
Monodisperse mesoporous silicon dioxide hollow nano-microsphere and preparation method Download PDFInfo
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- CN101857234B CN101857234B CN2010101960039A CN201010196003A CN101857234B CN 101857234 B CN101857234 B CN 101857234B CN 2010101960039 A CN2010101960039 A CN 2010101960039A CN 201010196003 A CN201010196003 A CN 201010196003A CN 101857234 B CN101857234 B CN 101857234B
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 239000004005 microsphere Substances 0.000 title claims abstract description 61
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 36
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 10
- 229920000136 polysorbate Polymers 0.000 claims abstract description 8
- 159000000000 sodium salts Chemical class 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 26
- 229960001866 silicon dioxide Drugs 0.000 claims description 24
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- 238000001354 calcination Methods 0.000 claims description 12
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 230000005855 radiation Effects 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 239000001103 potassium chloride Substances 0.000 claims description 8
- 235000011164 potassium chloride Nutrition 0.000 claims description 8
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 229920001214 Polysorbate 60 Polymers 0.000 claims description 4
- 229920002651 Polysorbate 85 Polymers 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 239000001818 polyoxyethylene sorbitan monostearate Substances 0.000 claims description 4
- 235000010989 polyoxyethylene sorbitan monostearate Nutrition 0.000 claims description 4
- 229940113124 polysorbate 60 Drugs 0.000 claims description 4
- 229940113171 polysorbate 85 Drugs 0.000 claims description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 4
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 3
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 3
- 229920000053 polysorbate 80 Polymers 0.000 claims description 3
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 claims description 3
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 3
- 235000015320 potassium carbonate Nutrition 0.000 claims description 3
- 239000004323 potassium nitrate Substances 0.000 claims description 3
- 235000010333 potassium nitrate Nutrition 0.000 claims description 3
- 239000001632 sodium acetate Substances 0.000 claims description 3
- 229960004249 sodium acetate Drugs 0.000 claims description 3
- 235000017281 sodium acetate Nutrition 0.000 claims description 3
- 208000006558 Dental Calculus Diseases 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 239000004317 sodium nitrate Substances 0.000 claims description 2
- 235000010344 sodium nitrate Nutrition 0.000 claims description 2
- 229940001516 sodium nitrate Drugs 0.000 claims description 2
- ZNRSXPDDVNZGEN-UHFFFAOYSA-K trisodium;chloride;sulfate Chemical group [Na+].[Na+].[Na+].[Cl-].[O-]S([O-])(=O)=O ZNRSXPDDVNZGEN-UHFFFAOYSA-K 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 10
- 239000002131 composite material Substances 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract description 2
- 239000000975 dye Substances 0.000 abstract description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 abstract 1
- 239000000969 carrier Substances 0.000 abstract 1
- 238000013270 controlled release Methods 0.000 abstract 1
- 239000002537 cosmetic Substances 0.000 abstract 1
- 239000012153 distilled water Substances 0.000 abstract 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 9
- 238000001914 filtration Methods 0.000 description 7
- 239000011259 mixed solution Substances 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 6
- 230000007062 hydrolysis Effects 0.000 description 5
- 238000006460 hydrolysis reaction Methods 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 3
- 239000011257 shell material Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 2
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 1
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 125000005587 carbonate group Chemical group 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000009415 formwork Methods 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 235000012204 lemonade/lime carbonate Nutrition 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 239000012766 organic filler Substances 0.000 description 1
- 239000008177 pharmaceutical agent Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
- UQMOLLPKNHFRAC-UHFFFAOYSA-N tetrabutyl silicate Chemical compound CCCCO[Si](OCCCC)(OCCCC)OCCCC UQMOLLPKNHFRAC-UHFFFAOYSA-N 0.000 description 1
- XQMTUIZTZJXUFM-UHFFFAOYSA-N tetraethoxy silicate Chemical group CCOO[Si](OOCC)(OOCC)OOCC XQMTUIZTZJXUFM-UHFFFAOYSA-N 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
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Abstract
The invention relates to a monodisperse mesoporous silicon dioxide hollow nano-microsphere and a preparation method, wherein the monodisperse mesoporous silicon dioxide hollow nano-microsphere comprises the following raw materials in parts by weight: 100 parts of ethyl orthosilicate, 40-60 parts of n-octyl amine, 5-15 parts of tween, 1.0-3.0 parts of inorganic sodium salt or potassium salt and 500 parts of distilled water. The mesoporous silicon dioxide hollow nano-microsphere is rapidly prepared under the action of ultrasonic waves, the method has simple process and quite short preparation time, and the mesoporous silicon dioxide hollow nano-microsphere prepared by the method has the grain diameter range of 40-200nm and the specific surface area of 980.4-1272.6m<2>/g, can be widely applied to the fields of preparation of low-dielectric-constant or light composite materials, controlled release of medicaments, carriers of catalysts, novel self-assembled materials and the like and also has wide application potentiality in the fields of dyes, cosmetics and the like.
Description
Technical field
The present invention relates to a kind of monodisperse mesoporous silica hollow Nano microsphere and preparation method, be specifically related to a kind of method of utilizing UW and dispersion agent under alkaline condition, to prepare monodisperse mesoporous silica hollow Nano microsphere fast.
Background of invention
The mesoporous silicon oxide hollow microsphere is that a kind of inside has the inorganic materials that has mesopore orbit on cavity, the spherical shell.Low because of its density, perveance is low, thermodynamic stability is high, have duct and higher specific surface area and can be widely used in absorption, stratographic analysis, the light composite material of support of the catalyst, medicine sustained release, toxic substance, the fields such as preparation of low dielectric constant composite.From people such as Kresge in 1992 on the Nature magazine reported first ordered mesoporous silica dioxide material of a kind of MCM-41 by name, the research of mesoporous silicon oxide becomes international focus rapidly.Because of the mesoporous silicon oxide hollow microsphere, especially mesoporous silicon oxide hollow Nano microsphere has bigger specific surface area, in recent years especially by various countries scientist broad research.The mesoporous silicon oxide hollow microsphere is mainly through adopting silicon source, template to utilize churned mechanically mode synthetic at present; Patent WO9740105 and CN101274246 are through being the silicon source with the tetraethoxy; Calcium carbonate powders is that template is prepared lime carbonate/silica core shell material earlier, obtains the silicon-dioxide hollow microsphere through calcining and Hydrogen chloride immersion treatment again.Except that adopting inorganic hard template; The preparation of silicon dioxide hollow microballon hollow microsphere also can be adopted soft template such as tensio-active agent organic fillers such as (like cetyl trimethylammonium bromide and 3-aminopropyl trimethoxysilane) or microemulsion; Described in patent CN1994879, CN1944251, CN1864846, CN101391776, CN101343065, CN101214965, CN101475183, CN101318550, CN1994879; But these method preparation times are longer; Generally reach several hours even tens of hours, the wide or serious agglomeration of product cut size distribution.Compare with other template; Utilize vesicle mold prepare the mesoporous silicon oxide hollow microsphere have the time short, efficient is high, reactant is few, advantage such as simple; Kosuge K, Cheng X, Liu S etc. have done a large amount of work in this field; With tetraethoxy or butyl silicate is the silicon source; With aminated compoundss such as NSC 9824 be template utilize the success of magnetic force rotor or mechanical stirring prepared pattern mesoporous silicon oxide hollow microsphere preferably, but these class methods all be with diluted acid as the catalytic hydrolysis agent, and the microspherulite diameter for preparing greatly, particle size distribution range broad, specific surface area be less.
Summary of the invention
The object of the present invention is to provide a kind of monodisperse mesoporous silica hollow Nano microsphere and preparation method; Under UW radiating condition; With inorganic sodium or sylvite is the hydrolysis auxiliary agent, is dispersion agent (improve the microspherulite diameter distribution range and can, suppress intergranular mutual reunion with the surface active that reduces microballoon in the preparation process) with the tween, prepares the silicon-dioxide hollow Nano microsphere that internal layer includes the NSC 9824 template fast; Place it in the retort furnace calcining then and remove the mesoporous silicon oxide hollow Nano microsphere of monodispersity that organic formwork forms, uniform grading, high-specific surface area; Technology of the present invention is simple, and preparation cycle is short, good product quality.
The quality group of the raw material of a kind of monodisperse mesoporous silica hollow Nano microsphere provided by the invention becomes:
100 parts of tetraethoxys
40～60 parts of NSC 9824s
5～15 parts of polysorbas20s
1.0～3.0 parts of inorganic sodium or sylvite
500 parts of zero(ppm) water
As the hydrolysis auxiliary agent, wherein sodium salt is sodium-chlor, sodium sulfate, yellow soda ash, SODIUMNITRATE, sodium-acetate with a kind of acids catalytic hydrolysis agent that replaces using always in inorganic sodium or the sylvite, and sylvite is Repone K, vitriolate of tartar, saltpetre, salt of wormwood, Potassium ethanoate; With the tween is dispersion agent, and wherein tween is a polysorbas20, polysorbate60, tween 80, a kind of in the polysorbate85;
The method of a kind of monodisperse mesoporous silica hollow Nano microsphere provided by the invention may further comprise the steps:
1) by metering tetraethoxy, NSC 9824, tween are added sodium salt or the sylvite dilute solution that mixes by metering after 10 minutes at thorough mixing under the UW radiation; Ultrasonic generator power is controlled to be 50W～100W; Preparation time is controlled to be 5 minutes, then the silicon-dioxide hollow Nano microsphere that internal layer comprises the NSC 9824 template is filtered, after washing with acetone, drying, promptly got to white products.
2) this silicon-dioxide hollow nano microsphere that comprises the NSC 9824 template is placed in the muffle furnace in 600～650 ℃ temperature lower calcination after 1 hour, promptly gets mesoporous silicon oxide hollow Nano microsphere with monodispersity, uniform grading, high-specific surface area.
The present invention is the hydrolysis auxiliary agent with inorganic sodium or sylvite, is that dispersion agent is prepared mesoporous silicon oxide hollow Nano microsphere fast with the tween under UW radiating condition, and this microballoon has the characteristics of monodispersity, uniform grading, high-specific surface area.Technology of the present invention is simple, and preparation cycle is short, good product quality.The mesoporous silicon oxide hollow Nano microsphere particle size range of processing through this method is that 40～200nm, specific surface area are up to 1272.6m
2/ g can be widely used in the field such as preparation, controlled delivery of pharmaceutical agents release, the carrier of catalyzer, novel self-assembled material of low-k or light composite material, and in fields such as dyestuff, makeup the widespread use potentiality is arranged also.
Description of drawings
Fig. 1 is the FESEM photo of mesoporous silicon oxide hollow Nano microsphere in the instance 3.
Fig. 2 is for containing the DTG figure of NSC 9824 template silicon-dioxide hollow Nano microsphere in the instance 3.
Fig. 3 is the little angle XRD figure of mesoporous silicon oxide hollow Nano microsphere in the instance 3.
Fig. 4 is the N of mesoporous silicon oxide hollow Nano microsphere in the instance 3
2Absorption/desorption figure.
Embodiment
Instance 1: with 100g tetraethoxy, 40g NSC 9824,5g polysorbas20 thorough mixing 10 minutes under the UW radiation; Join in the above-mentioned mixed solution after then 1.0g sodium-chlor and 500g zero(ppm) water being mixed; Ultrasonic generator power is controlled to be 50W; Ultrasonic time is controlled to be 5 minutes, then with promptly getting the silicon-dioxide hollow Nano microsphere that comprises the NSC 9824 template after white products filtration, washing with acetone, the drying.This silicon-dioxide hollow Nano microsphere that comprises the NSC 9824 template was placed in the muffle furnace in 600～650 ℃ temperature lower calcination after 1 hour, promptly get have monodispersity, particle diameter is about between 40～110nm, specific surface area is 980.4m
2The mesoporous silicon oxide hollow Nano microsphere of/g.
Instance 2: with 100g tetraethoxy, 55g NSC 9824,10g tween 80 thorough mixing 10 minutes under the UW radiation; Join in the above-mentioned mixed solution after then 1.5g saltpetre and 500g zero(ppm) water being mixed; Ultrasonic generator power is controlled to be 50W; Ultrasonic time is controlled to be 5 minutes, then with promptly getting the silicon-dioxide hollow Nano microsphere that comprises the NSC 9824 template after white products filtration, washing with acetone, the drying.This silicon-dioxide hollow Nano microsphere that comprises the NSC 9824 template was placed in the muffle furnace in 600～650 ℃ temperature lower calcination after 1 hour, promptly get have monodispersity, particle diameter is about between 60～200nm, specific surface area is 1210.6m
2The mesoporous silicon oxide hollow Nano microsphere of/g.
Instance 3: with 100g tetraethoxy, 64g NSC 9824,8g polysorbas20 thorough mixing 10 minutes under the UW radiation; Join in the above-mentioned mixed solution after then 2.5g salt of wormwood and 500g zero(ppm) water being mixed; Ultrasonic generator power is controlled to be 100W; Ultrasonic time is controlled to be 5 minutes, then with promptly getting the silicon-dioxide hollow Nano microsphere that comprises the NSC 9824 template after white products filtration, washing with acetone, the drying.This silicon-dioxide hollow Nano microsphere that comprises the NSC 9824 template was placed in the muffle furnace in 600～650 ℃ temperature lower calcination after 1 hour, promptly get have monodispersity, particle diameter is about between 50～150nm, specific surface area is 1272.6m
2The mesoporous silicon oxide hollow Nano microsphere of/g.
Fig. 1 is the FESEM photo of mesoporous silicon oxide hollow Nano microsphere in the instance 3, from figure, can obviously find out, product cut size is about between 50～150nm, is separated into monodispersity, structure is tangible hollow structure (shown in arrow and an illustration); Fig. 2 is for containing the DTG figure of NSC 9824 template silicon-dioxide hollow Nano microsphere in the instance 3; Have by figure; Obviously there are three weight loss rate peaks in the silicon-dioxide hollow Nano microsphere that contains the NSC 9824 template; Can know through analyzing: the peak of 105 ℃ of correspondences is that free-water produces in the sample, and the peak of 249 ℃ of correspondences is that NSC 9824 is caused, and the peak of 424 ℃ of correspondences is that polysorbas20 is caused.Can know also that by figure after calcining temperature was 600～650 ℃, organism was removed fully; Fig. 3 is the little angle XRD figure of mesoporous silicon oxide hollow Nano microsphere in the instance 3, can know that from figure at 2 θ be diffraction peak of appearance in 2.88 o'clock, and the spherical shell of the product of this provable gained is a meso-hole structure; Fig. 4 is the N of mesoporous silicon oxide hollow Nano microsphere in the instance 3
2Absorption/desorption figure, curve presents hysteresis among the figure, and this explanation is tangible meso-hole structure through the mesoporous silicon oxide hollow Nano microsphere of the present invention's preparation; This also with Fig. 3 in little angle XRD test result consistent; Also can know that by figure the specific surface area of microballoon is very high simultaneously, be 1272.6m
2/ g (this hollow structure with microballoon is corresponding), and the surface mesoporous distribution of spherical shell is the center with 1.2nm, and scope is 0.5nm～2.5nm, and distribution range is narrow.
Instance 4: with 100g tetraethoxy, 60g NSC 9824,10g polysorbate60 thorough mixing 10 minutes under the UW radiation; Join in the above-mentioned mixed solution after then 3.0g sodium-acetate and 500g zero(ppm) water being mixed; Ultrasonic generator power is controlled to be 100W; Ultrasonic time is controlled to be 5 minutes, then with promptly getting the silicon-dioxide hollow Nano microsphere that comprises the NSC 9824 template after white products filtration, washing with acetone, the drying.This silicon-dioxide hollow Nano microsphere that comprises the NSC 9824 template was placed in the muffle furnace in 600～650 ℃ temperature lower calcination after 1 hour, promptly get have monodispersity, particle diameter is about between 70～160nm, specific surface area is 1063.2m
2The mesoporous silicon oxide hollow Nano microsphere of/g.
Instance 5: with 100g tetraethoxy, 40g NSC 9824,10g polysorbate85 thorough mixing 10 minutes under the UW radiation; Join in the above-mentioned mixed solution after then 2.0g sodium sulfate and 500g zero(ppm) water being mixed; Ultrasonic generator power is controlled to be 70W; Ultrasonic time is controlled to be 5 minutes, then with promptly getting the silicon-dioxide hollow Nano microsphere that comprises the NSC 9824 template after white products filtration, washing with acetone, the drying.This silicon-dioxide hollow Nano microsphere that comprises the NSC 9824 template was placed in the muffle furnace in 650 ℃ temperature lower calcination after 1 hour, promptly get have monodispersity, particle diameter is about between 40～180nm, specific surface area is 1147.8m
2The mesoporous silicon oxide hollow Nano microsphere of/g.
Instance 6: with 100g tetraethoxy, 48g NSC 9824,15g polysorbate60 thorough mixing 10 minutes under the UW radiation; Join in the above-mentioned mixed solution after then 1.0g Potassium ethanoate and 500g zero(ppm) water being mixed; Ultrasonic generator power is controlled to be 50W; Ultrasonic time is controlled to be 5 minutes, then with promptly getting the silicon-dioxide hollow Nano microsphere that comprises the NSC 9824 template after white products filtration, washing with acetone, the drying.This silicon-dioxide hollow Nano microsphere that comprises the NSC 9824 template was placed in the muffle furnace in 600～650 ℃ temperature lower calcination after 1 hour, promptly get have monodispersity, particle diameter is about between 60～190nm, specific surface area is 996.1m
2The mesoporous silicon oxide hollow Nano microsphere of/g.
Instance 7: with 100g tetraethoxy, 55g NSC 9824,11g polysorbate85 thorough mixing 10 minutes under the UW radiation; Join in the above-mentioned mixed solution after then 2.0g Repone K and 500g zero(ppm) water being mixed; Ultrasonic generator power is controlled to be 90W; Ultrasonic time is controlled to be 5 minutes, then with promptly getting the silicon-dioxide hollow Nano microsphere that comprises the NSC 9824 template after white products filtration, washing with acetone, the drying.This silicon-dioxide hollow Nano microsphere that comprises the NSC 9824 template was placed in the muffle furnace in 600～650 ℃ temperature lower calcination after 1 hour, promptly get have monodispersity, particle diameter is about between 70～170nm, specific surface area is 1084.6m
2The mesoporous silicon oxide hollow Nano microsphere of/g.
Claims (3)
1. the preparation method of a monodisperse mesoporous silica hollow Nano microsphere, the quality group of its raw material becomes:
It is characterized in that may further comprise the steps:
1) by metering tetraethoxy, NSC 9824, tween are added sodium salt or the sylvite dilute solution that mixes by metering after 10 minutes at thorough mixing under the UW radiation; Ultrasonic generator power is controlled to be 50～100W; Preparation time is controlled to be 5 minutes, then the silicon-dioxide hollow Nano microsphere that includes the NSC 9824 template is filtered, after washing with acetone, drying, promptly got to white products;
2) this silicon-dioxide hollow Nano microsphere that comprises the NSC 9824 template is placed in the muffle furnace in 600～650 ℃ temperature lower calcination after 1 hour, promptly gets the mesoporous silicon oxide hollow Nano microsphere of tool monodispersity, uniform grading, high-specific surface area.
2. method according to claim 1 is characterized in that described inorganic sodium is sodium-chlor, sodium sulfate, yellow soda ash, SODIUMNITRATE or sodium-acetate; Sylvite is Repone K, vitriolate of tartar, saltpetre, salt of wormwood or Potassium ethanoate.
3. method according to claim 1 is characterized in that described tween is a kind of in polysorbas20, polysorbate60, tween 80 or the polysorbate85.
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| CN102583404A (en) * | 2012-03-15 | 2012-07-18 | 天津大学 | Mesoporous silicon dioxide nanometer particle and preparation method |
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| CN103482634B (en) * | 2013-09-09 | 2015-07-01 | 辽宁石油化工大学 | Preparation method of silicon-based dual mesoporous material |
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| CN111620342B (en) * | 2020-06-03 | 2021-11-19 | 南京特粒材料科技有限公司 | Small-size monodisperse hollow silica microsphere and preparation method and application thereof |
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