CN102951648B - Preparation method of nano silicon dioxide - Google Patents
Preparation method of nano silicon dioxide Download PDFInfo
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- CN102951648B CN102951648B CN201110255574.XA CN201110255574A CN102951648B CN 102951648 B CN102951648 B CN 102951648B CN 201110255574 A CN201110255574 A CN 201110255574A CN 102951648 B CN102951648 B CN 102951648B
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- active agent
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Abstract
The invention relates to a preparation method of nano silicon dioxide, which comprises the following steps: carrying out hydrolytic condensation on tetraethylorthosilicate by using alanine as a structure guide agent to obtain a silicon dioxide crystal seed suspension; preparing a low-concentration crystal seed suspension; adding sodium lauryl sulfate and sodium silicate; and slowly and dropwisely adding a sulfuric acid solution to regulate the pH value of the system so that the silicon dioxide generated by the hydrolytic condensation of silicate grows on the external surface of the silicon dioxide crystal seed, thereby obtaining the silicon dioxide spheres. Nano silicon dioxide with different specific areas and pore structures can be prepared by regulating the surfactant concentration, aging temperature and roasting temperature; and the specific area is 193-305 m<3>/g, the pore volume is 1.25-1.68 cm<3>/g, and the pore size is 17-34nm. Compared with the existing preparation method, the nano silicon dioxide prepared by the method provided by the invention has the advantages of more uniform particle size and more centralized pore size distribution, thereby having favorable application prospects.
Description
Technical field
A preparation method for nano silicon, belongs to the technology of preparing of inorganic nano material, is specifically related to a kind ofly taking alkali-metal silicate as silicon source, prepares the method for nanometer grade silica.
Background technology
Nano silicon is unformed white powder, is a kind of nontoxic, tasteless and free of contamination nonmetal functional materials, can be widely used as support of the catalyst, separating agent, sorbent material and chemical-biological sensing material etc.For these application, specific surface area, pore volume and pore size distribution that the key factor that affects nano silicon performance is sample.Therefore, in the preparation process of nano silicon, how to control its specific surface area and pore structure, become an important problem.
About the technology of preparing of silicon-dioxide, Chinese patent 02149782.6 discloses " a kind of preparation method of high-dispersion nano silicon-dioxide ", the method is burnt oxygen, hydrogen and organohalosilanes according to certain ratio, the water that halosilanes and burning generate is at high temperature hydrolyzed, condensation reaction, obtains product.The shortcoming of the method is expensive raw material price, and cost is higher.Chinese patent 02132723.8 discloses " process for preparing nano silicone dioxide by adopting two-step carbonization reaction ", and this technique is with sodium silicate aqueous solution and CO
2for raw material, in super gravity field reactor, carry out carbonation reaction, carbonation reaction liquid enters subsequently hot water and separates out in groove, can separate out nano silicon.This technique is had relatively high expectations to reaction conditions, and processing unit is loaded down with trivial details, and cost is higher.Sol-gel method is the conventional method of preparing silica spheres, and its operation is comparatively simple, and applicability is better.Chinese patent 95102373.X discloses " a kind of preparation method of silicon dioxide powder with controllable nanon size ", and it is raw material that the method adopts tetraethoxy, generates silica dioxide gel by hydrolysis, then drying, roasting obtain nano level superfine silicon-dioxide.But the circularity of product prepared by traditional sol-gel method, monodispersity and size distribution are poor, the shortcoming of the method is also that raw material tetraethoxy is expensive simultaneously.Chinese patent 201010126295.9 discloses " method of the controlled mono-dispersed nano silica dioxide granule of a kind of easy preparation size ", the method is added kinds of surface promoting agent and is prepared microemulsion system, ammonification water-initiated polymerization again after adding positive silicic acid lipid to mix, nanometer ball is precipitated out with acetone breakdown of emulsion, washing is removed tensio-active agent and is obtained product.But the method needs to use a large amount of organism in preparation process, reclaim more difficultly, cost is high and can be to environment.
In order to meet the nanometer silicon dioxide of the pore structures such as preparation certain pore size, pore volume, specific surface area the needs that reduce production costs, can effectively regulate the structural parameter of nano silicon, need to be taking cheap alkalimetal silicate as raw material, in time, by selecting different surfactant concentrations, aging temperature and maturing temperature, preparation has the nano silicon of different specific surface areas and pore structure.
Summary of the invention
The technical problem to be solved in the present invention is: overcome the deficiencies in the prior art, a kind of preparation technology of novel silicon-dioxide is provided, this kind of technique is by selecting different surfactant concentrations, aging temperature and maturing temperature to realize the control to nano silicon specific surface area and pore structure, nano silicon uniform particle diameter, the pore size distribution prepared with scheme disclosed by the invention are concentrated, and meet the needs as silica supports.
The present invention solves the technical scheme that its technical problem takes: a kind of preparation method of nano silicon, is characterized in that comprising the following steps:
1, in the distilled water that is dissolved with L-Ala, add tetraethoxy, and stir 24h at 50～60 DEG C, make SiO
2crystal seed suspension;
2, get silica-seed suspension, after adding distil water dilution, then in diluent, add tensio-active agent at 30～50 DEG C, uniform stirring makes it to dissolve completely, then adds water glass vigorous stirring to obtain homogeneous phase solution;
3, at 20～30 DEG C, in homogeneous phase solution, dropwise drip dilute sulphuric acid, drop to 7 to system pH, and by gained silica dioxide gel at 20～60 DEG C in encloses container after aging 18h, through washing, filter, the dry nano silicon that obtains;
4, the nano silicon of step 3 gained is obtained to finished product nano silicon at 550～670 DEG C of roasting 3～5h.
In described step 1, the ratio of the amount of substance of distilled water, tetraethoxy and L-Ala is n (H
2o): n (tetraethoxy): n (L-Ala)=153: 1: 0.04.
In described step 2, get 22 times of appropriate silica-seed suspension adding distil water dilutions.
Tensio-active agent described in step 2 is the one in sodium lauryl sulphate, triblock polymer P123 and cetyl trimethylammonium bromide, and the ratio of the amount of substance of water, tensio-active agent and water glass is n (H
2o): n (tensio-active agent): n (water glass)=111: 0.01～0.3: 1.
In step 2, tensio-active agent is cetyl trimethylammonium bromide, and the ratio of the amount of substance of water, tensio-active agent and water glass is n (H
2o): n (tensio-active agent): n (water glass)=111: 0.012: 1.
Aging temperature described in step 3 is 25 DEG C.
Maturing temperature described in step 4 is 650 DEG C.
Finished product nano silicon specific surface area described in step 4 is 193～305m
3/ g, aperture is 17～34nm, pore volume is 1.25～1.68cm
3/ g, piles up hole taking mesoporous as main.
The present invention is under the existence of structure directing agent L-Ala, and hydrolyzing condensation of ethyl silicate generates SiO
2crystal seed, obtains SiO
2crystal seed suspension.Through the SiO of dilution preparation lower concentration
2seed-solution, adds tensio-active agent and alkalimetal silicate, slowly drips sulphuric acid soln regulation system pH value, and pH is within 7 o'clock, to be dropping terminal.
In dropping process, the SiO that alkalimetal silicate hydrolytic condensation generates
2be attached to SiO
2thereby crystal seed outside surface evenly growth obtains silica spheres.The gel of gained through aging, washing, filter, dry and roasting obtains product.
Realize the control to nano silicon specific surface area and pore structure by selecting different surfactant concentrations, aging temperature and maturing temperature.The impact that single factors vary in surfactant concentration, aging temperature and maturing temperature causes is:
When the proportioning of reactant is n (H
2o): n (tensio-active agent): n (water glass)=50: (0.001～0.1): 1, temperature of reaction is 25 DEG C, when aging temperature is 25 DEG C, because of the difference of surfactant concentration using, prepared nano silicon specific surface area after 550 DEG C of roastings is 250～400m
2/ g, aperture is 15～30nm, pore volume is 1.0～1.5cm
3/ g.Along with the increase of surfactant concentration, the specific surface area of nano silicon increases, and aperture and pore volume reduce.
When the proportioning of reactant is n (H
2o): n (tensio-active agent): n (water glass)=50: 0.005: 1, when temperature of reaction is 25 DEG C, within the scope of 20～60 DEG C, regulate aging temperature, prepared nano silicon specific surface area after 550 DEG C of roastings is 100～250m
2/ g, aperture is 15～28nm, pore volume is 0.5～1.4cm
3/ g.Along with the increase of aging temperature, the specific surface area of product reduces, and pore volume and aperture increase.
When the proportioning of reactant is n (H
2o): n (tensio-active agent): n (water glass)=50: 0.005: 1, temperature of reaction is that 25 DEG C, aging temperature are while being 25 DEG C, within the scope of 550～670 DEG C, regulate maturing temperature, after high-temperature roasting, the specific surface area of nano silicon is 150～260m
2/ g, aperture is 14～35nm, pore volume is 0.5～2.0cm
3/ g.Along with the increase of maturing temperature, the specific surface area of sample reduces, and pore volume and aperture increase.
In the process of adjusting pH, sulfuric acid dropwise adds in system slowly, and system keeps high-speed stirring, has avoided the local acidity of system too high, thereby has made SiO
2crystal seed is progressively grown and is effectively prevented secondary nucleation.
Compared with prior art, the beneficial effect that the preparation method of a kind of nano silicon of the present invention has is:
1, technique of the present invention is simple, and raw material is relatively cheap, and without expensive device, running cost is low, in the washes of product, contains Na
+, SO
4 2-and tensio-active agent, Na
+, SO
4 2-recoverable, tensio-active agent can be degraded by biological process, can not produce secondary pollution.
2, first the present invention prepares SiO
2crystal seed, and as core, the SiO that hydrolyzed silicate condensation generates
2be attached to its outside surface and evenly grow, thereby the nano silicon spherolite footpath of preparation is more even, pore size distribution is more concentrated.
3, specific surface area and the pore structure that in the present invention, can control by the concentration of reconciliation statement surface-active agent, aging temperature and maturing temperature product, the finished product nano silicon specific surface area of gained is 193～305m
3/ g, aperture is 17～34nm, pore volume is 1.25～1.68cm
3/ g, piles up hole taking mesoporous as main, can meet completely as reactant carrier or in other side and apply.
Brief description of the drawings
Fig. 1 is embodiment 7 gained nanometer SiO
2the nitrogen adsorption desorption curve of sample.
Fig. 2 is embodiment 7 gained nanometer SiO
2the pore size distribution curve of sample.
Embodiment
Embodiment 1
54.6mg L-Ala (6.1 × 10
-4mol) be dissolved in 41.4g distilled water (2.3mol), add 3.13g tetraethoxy (0.015mol), whole reaction system, in 50～60 DEG C of stirring 24h, obtains silica-seed suspension.
Thermostatic bath hierarchy of control temperature, at 25 DEG C, measures 2ml suspension, and adding distil water, to 44ml (amount of substance is 2.44mol), dilutes 22 times.(molar mass 5800g/mol, amount of substance is 5.1 × 10 at 30～40 DEG C, to add 2.96g triblock polymer P123
-4mol), stir 20min and make it to dissolve completely, then add 6.24g nine water water glass (amounting to water glass is 0.022mol), vigorous stirring 30min forms homogeneous phase solution.
Keep whipped state, at 20～30 DEG C, in homogeneous phase solution, dropwise drip the sulfuric acid of 50wt% until the pH=7 of solution forms silica dioxide gel.The silica dioxide gel obtaining is aging 18h under sealed environment, 20～25 DEG C of aging temperatures.Gel after aging after filtration, washing and dry after, obtain product 550 DEG C of roastings.The specific surface area of sample and pore structure data are in table 1.
Embodiment 2
The triblock polymer P123 quality adding in reaction system is 1.48g (2.55 × 10
-4mol), all the other steps are identical with method described in embodiment 1.The specific surface area of sample and pore structure data are in table 1.
Embodiment 3
54.6mg L-Ala is dissolved in 41.4g distilled water, adds 3.13g tetraethoxy, and whole reaction system, in 50～60 DEG C of stirring 24h, obtains silica-seed suspension.
Thermostatic bath hierarchy of control temperature is 25 DEG C, measures 2ml suspension, 22 times of adding distil water dilutions.At 40～50 DEG C, add 0.093g cetyl trimethylammonium bromide (2.6 × 10
-4mol), stir 20min and make it to dissolve completely, then add 6.24g water glass, vigorous stirring 30min forms homogeneous phase solution.Keep whipped state, dropwise drip the sulfuric acid of 50wt% until the pH=7 of solution forms silica dioxide gel.The silica dioxide gel obtaining is aging 18h under sealed environment, 25 DEG C of aging temperatures.Gel after aging after filtration, washing and dry after, obtain product 550 DEG C of roastings.The specific surface area of sample and pore structure data are in table 1.
Embodiment 4
The aging temperature of silica dioxide gel is 40 DEG C, and all the other steps are identical with method described in embodiment 3.The specific surface area of sample and pore structure data are in table 1.
Embodiment 5
The aging temperature of silica dioxide gel is 60 DEG C, and all the other steps are identical with method described in embodiment 3.The specific surface area of sample and pore structure data are in table 1.
Embodiment 6
The maturing temperature of sample is 600 DEG C, and all the other steps are identical with method described in embodiment 3.The specific surface area of sample and pore structure data are in table 1.
Embodiment 7
The maturing temperature of sample is 650 DEG C, and all the other steps are identical with method described in embodiment 3.The specific surface area of sample and pore structure data are in table 1.
The performance characterization of table 1 embodiment 1～7 products obtained therefrom
Use for meeting as reaction carriers, embodiment 7 is in embodiment 1～7 Chinese style preferred plan.
By Fig. 1 embodiment 7 gained nanometer SiO
2the nitrogen adsorption desorption curve of sample is known, and it is stable, good that the silicon-dioxide of this routine gained shows in nitrogen adsorption, by Fig. 2 embodiment 7 gained nanometer SiO
2the pore size distribution of the known sample of pore size distribution curve of sample is comparatively concentrated.
For exploring the application kind of tensio-active agent, carry out embodiment 8～10.
Embodiment 8
Tensio-active agent is selected sodium lauryl sulphate (molar mass 288g/mol), and quality is that 0.6g (amount of substance is 0.0022mol) all the other steps and amounts of components are identical with method described in embodiment 7.Sodium lauryl sulphate is 0.1: 1 with the ratio of the amount of substance of water glass.
Embodiment 9
Tensio-active agent is selected sodium lauryl sulphate, and quality is 1.26g (amount of substance is 0.0044mol), and all the other steps and amounts of components are identical with method described in embodiment 7.Sodium lauryl sulphate is 0.2: 1 with the ratio of the amount of substance of water glass.
Embodiment 10
Tensio-active agent is selected sodium lauryl sulphate, and quality is 0.06g, and all the other steps and amounts of components are identical with method described in embodiment 7.Sodium lauryl sulphate is 0.01: 1 with the ratio of the amount of substance of water glass.
The above, be only preferred embodiment of the present invention, is not the restriction of invention being made to other form, and any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the equivalent embodiment of equivalent variations.But every technical solution of the present invention content that do not depart from, any simple modification, equivalent variations and the remodeling above embodiment done according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (7)
1. a preparation method for nano silicon, is characterized in that comprising the following steps:
1.1, in the distilled water that is dissolved with L-Ala, add tetraethoxy, and stir 24h at 50～60 DEG C, make silica-seed suspension;
1.2, get silica-seed suspension, after adding distil water dilution, then in diluent, add tensio-active agent uniform stirring to make it to dissolve completely at 30～50 DEG C, then add water glass, vigorous stirring obtains homogeneous phase solution;
1.3, at 20～30 DEG C, in homogeneous phase solution, dropwise drip dilute sulphuric acid, to system pH=7, obtain silica dioxide gel, gained silica dioxide gel after aging 18h, is obtained to nano silicon through washing, filtration, drying process at 20～60 DEG C in encloses container;
1.4, by step 1.3 gained nano silicon at 550～670 DEG C of roasting 3～5h, obtain finished product nano silicon;
Tensio-active agent described in step 1.2 is the one in sodium lauryl sulphate, triblock polymer P123 and cetyl trimethylammonium bromide, and the ratio of the amount of substance of water, tensio-active agent and water glass is n (H
2o): n (tensio-active agent): n (water glass)=111:0.01～0.3:1.
2. the preparation method of a kind of nano silicon according to claim 1, is characterized in that: in step 1.1, the ratio of the amount of substance of distilled water, tetraethoxy and L-Ala is n (H
2o): n (tetraethoxy): n (L-Ala)=153:1:0.04.
3. the preparation method of a kind of nano silicon according to claim 1, is characterized in that: in step 1.2, get 22 times of appropriate silica-seed suspension adding distil water dilutions.
4. the preparation method of a kind of nano silicon according to claim 1, is characterized in that: the tensio-active agent described in step 1.2 is cetyl trimethylammonium bromide, and the ratio of the amount of substance of water, tensio-active agent and water glass is n (H
2o): n (tensio-active agent): n (water glass)=111:0.012:1.
5. the preparation method of a kind of nano silicon according to claim 1, is characterized in that: the aging temperature described in step 1.3 is 25 DEG C.
6. the preparation method of a kind of nano silicon according to claim 1, is characterized in that: the maturing temperature described in step 1.4 is 650 DEG C.
7. the preparation method of a kind of nano silicon according to claim 1, is characterized in that: the finished product nano silicon specific surface area described in step 1.4 is 193～305m
3/ g, aperture is 17～34nm, pore volume is 1.25～1.68cm
3/ g, piles up hole taking mesoporous as main.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104556071B (en) * | 2014-12-29 | 2017-01-04 | 上海新安纳电子科技有限公司 | A kind of preparation method and applications of porous silica |
| CN104888531B (en) * | 2015-06-02 | 2016-11-02 | 江苏华强新能源科技有限公司 | A kind of preparation technology of gas-turbine plant nanoscale composite filter material |
| CN108017061B (en) * | 2017-12-06 | 2020-12-08 | 上海应用技术大学 | Method for preparing large-specific-surface-area nano SiO by using water glass2Method (2) |
| CN109734347A (en) * | 2018-12-13 | 2019-05-10 | 中国铁道科学研究院集团有限公司铁道建筑研究所 | A kind of enhanced alkali-free quick-coagulant of nanosized seeds and preparation method thereof |
| CN112226221B (en) * | 2020-10-19 | 2022-03-01 | 河南大学 | Nano silicon dioxide oil displacement agent and preparation method and application thereof |
| CN114873598B (en) * | 2022-06-09 | 2023-09-22 | 福建省瞄小懒科技有限责任公司 | Silicon dioxide and preparation method thereof |
| CN115924924A (en) * | 2022-08-23 | 2023-04-07 | 河南大学 | Hollow spherical silicon dioxide with adjustable specific surface area and preparation method and application thereof |
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