CN101891211A - Silicon dioxide mesoporous material with multilayer sleeve structure and preparation thereof - Google Patents
Silicon dioxide mesoporous material with multilayer sleeve structure and preparation thereof Download PDFInfo
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Abstract
The invention discloses a silicon dioxide mesoporous material with a multilayer sleeve structure and preparation thereof. The silicon dioxide mesoporous material is a mesoporous silicon dioxide hollow tubular material with the multilayer sleeve structure, wherein the length of the hollow tubular material is between 3 and 10mu m, the outer diameter is between 150 and 200nm, the inner diameter is between 50 and 60nm, and the specific surface area is between 500 and 600m<2>g<-1>; and amidocyanogen is uniformly distributed on the mesoporous wall. The silicon dioxide mesoporous material is obtained by using acid or salt of chiral anionic surfactant as a main structure directing agent, and in the presence of alkali or acid, using alkaline silane with amidocyanogen as a co-structure directing agent and organic silane as a silicon source. The silicon dioxide mesoporous material has wide application prospect in medicament separation, medicament load, catalysis and other fields.
Description
Technical field
The present invention relates to a kind of inorganic porous material, particularly a kind of SiO 2 mesoporous materials and preparation method thereof with multilayer sleeve structure.
Background technology
Mesoporous material has big specific surface area and pore volume, adjustable pore structure, adjustable aperture, the surface properties that can modify and the pattern that can control or the like, thereby in separation, catalysis, sensing, medicament slow release and as the every field such as template of synthetic other materials very large application potential is arranged all.The nano-tube of meso-hole structure is because it has three kinds of surface-area: the internal surface of the internal surface of nanotube, outside surface and mesopore orbit makes it become the material that using value is more arranged.
Up to the present, document Nano.Lett., 1,145 (2001); Chem.Commun., 2343 (2000); J. Am.Chem.Soc., 123,8785 (2001); Chem.Mater., 19,1329 (2007) reported by the sol-gel clone method and synthesized the mono-layer tube arm nano-tube material that wall does not have the duct; Document J. Chem.Soc.PerkinTrans., 2,1289 (1999); Chem.Commun., 1477 (1998); Langmuir, 16,1643 (2000); Angew.Chem.Int.Ed., 41,2988 (2002); Reported by the sol-gel clone method and synthesized the nano-tube material that wall does not have the sleeve structure in duct.Adv.Funct.Mater., 18,541-550 (2008) has reported that with anion surfactant be template, the quaternary amine ammonium salt is to help structure directing agent to synthesize the mesoporous silicon dioxide nano tube material of mono-layer tube arm under 30 ℃.But these materials are not owing to having meso-hole structure or specific surface area little, and application is restricted.
Summary of the invention
The objective of the invention is to overcome defective of the prior art, SiO 2 mesoporous materials and preparation and application with multilayer sleeve structure are provided.
The constitutional features of SiO 2 mesoporous materials of the present invention is as follows:
It is the mesoporous silicon oxide hollow tubular material with multilayer sleeve structure, and wherein, the length of hollow tubular material is 3-10 μ m, and outside diameter is 150-200nm, and interior diameter is 50-60nm, and specific surface area is 500-600m
2g
-1, uniform distribution amido on the mesoporous wall.
Further, the mesoporous aperture of described mesoporous material is 3-4nm, and pore volume is 300-600mm
3g
-1
SiO 2 mesoporous materials of the present invention is that salt with the acid of chirality anion surfactant or chirality anion surfactant is as the main structure directed agents, in the presence of alkali or acid, for helping structure directing agent, and is the SiO 2 mesoporous materials with multilayer sleeve pattern of silicon source reaction acquisition with the organosilane with the basic silane of band amido.
Specifically comprise the following steps:
1) preparation of colloidal sol:
The aqueous solution of acid, deionized water and the alkali of chirality anion surfactant is at room temperature mixed preparation colloidal sol;
Perhaps salt, deionized water and the inorganic aqueous acid with the chirality anion surfactant at room temperature mixes preparation colloidal sol;
2) colloidal sol that step 1 is obtained stirred 10-15 hour under-1～1 ℃, and the basic silane that adds the band amido earlier helps structure directing agent, adds organosilane again, leaves standstill 1-2 days under-1～1 ℃ after mixing; Preferred 0 ℃ of the temperature of this step.
3) obtain to have the mesoporous silicon oxide hollow tubular material of multilayer sleeve structure through separation, washing, drying and suction filtration.
In the step 1, the acid of chirality anion surfactant: deionized water: alkali: the basic silane of band amido: the mol ratio of organosilane is 1: 500-4000: 0.8-0.9: 2.0-2.5: 5-10;
In the step 1, the salt of chirality anion surfactant: deionized water: mineral acid: the basic silane of band amido: the mol ratio of organosilane is 1: 500-4000: 0.1-0.2: 2.0-2.5: 5-10;
The acid of the chirality anion surfactant that the present invention uses is replaced-L-L-Ala (C as N-alkyl acyl
n-L-AlaA) or N-alkyl acyl for-D-L-Ala (C
n-D-AlaA), its structural formula is as follows:
Wherein, R
1Be C
nH
2n+1, n=14 or 16; A is COO
-Wherein have left-hand to: N-tetradecyl acyl for-L-L-Ala, N-hexadecyl acyl for-L-L-Ala and right-hand lay: N-tetradecyl acyl for-D-L-Ala, N-hexadecyl acyl for-D-L-Ala.
The salt of chirality anion surfactant used in the present invention is: N-alkyl acyl replaces-L-L-Ala salt (C
n-L-AlaS) or N-alkyl acyl for-D-L-Ala salt (C
n-D-AlaS), its structural formula is as follows:
Wherein, R
1Be C
nH
2n+1, n=14 or 16; A is COO
-; B is Na
+, K
+, NH
4 +Wherein have left-hand to: N-tetradecyl acyl for-L-L-Ala sylvite, N-hexadecyl acyl for-L-L-Ala sylvite, N-tetradecyl acyl for-L-L-Ala sodium salt, N-hexadecyl acyl for-L-L-Ala sodium salt, N-tetradecyl acyl for-L-L-Ala ammonium salt, N-hexadecyl acyl for-L-L-Ala ammonium salt etc.; Right-hand lay: N-tetradecyl acyl for-D-L-Ala sylvite, N-hexadecyl acyl for-D-L-Ala sylvite, N-tetradecyl acyl for-D-L-Ala sodium salt, N-hexadecyl acyl for-D-L-Ala sodium salt, N-tetradecyl acyl for-D-L-Ala ammonium salt, N-hexadecyl acyl for-D-L-Ala ammonium salt etc.
Mineral acid used in the present invention is sulfuric acid, hydrochloric acid, Hydrogen bromide or nitric acid.
Alkali used in the present invention is sodium hydroxide, potassium hydroxide or short chain small molecule amine, and wherein the short chain small molecule amine has ammoniacal liquor, methylamine, ethamine etc.
The structure directing agent that helps used in the present invention is the basic silane of band amido, and its structural formula is shown below:
(R
1O)
3Si—R—NH
2
Wherein, R
1Be C
1-C
4Straight chain, branched chain alkyl or hydrogen atom; R is C
1-C
4Straight chain or branched chain alkyl, 3-aminopropyl trimethoxysilane, 3-aminopropyl triethoxysilane, 4-ammonia butyl trimethoxy silane etc. are wherein arranged.
Organosilane used in the present invention is shown below:
(R
1O)
m——Si——R
n
Wherein, the integer of m=2-4, R
1Be C
1-C
4Straight chain, branched chain alkyl or hydrogen atom; The integer of n=0-2, R are C
1-C
4Straight chain or branched chain alkyl, m+n=4.Tetramethoxy-silicane, tetraethoxysilane, tetrapropoxysilane, tetraisopropoxysilan, four butoxy silanes are wherein arranged, and also can be dimethoxy dimethylsilane, trimethoxymethylsila,e, dimethoxy di-isopropyl silane etc.
Structural representation with SiO 2 mesoporous materials of multilayer sleeve structure of the present invention is seen Fig. 1, i.e. basic silane conduct with amido helps structure directing agent that anion surfactant and organosilane are combined, and has formed the SiO 2 mesoporous materials with multilayer sleeve structure.
The SiO 2 mesoporous materials of multilayer sleeve structure of the present invention can be applicable to fields such as separation, catalysis, medicament slow release.
The SiO 2 mesoporous materials of multilayer sleeve structure of the present invention is compared with the silicon-dioxide tubulose material in existing non-hole, has bigger serface, big porosity, mesopore orbit evenly with advantages such as organo-functional groups; Compare with the tubulose mesoporous material of individual layer tube wall and to have advantages such as multistage surface, specific surface area is big, adsorptive capacity is big.Therefore, in catalysis, drug loading and separation, make support of the catalyst and hard template method and prepare in the fields such as mesoporous material and have wide practical use.
Description of drawings:
Fig. 1 is the structural representation with SiO 2 mesoporous materials of multilayer sleeve structure.
Fig. 2 is the sem photograph of the SiO 2 mesoporous materials of the multilayer sleeve structure that obtains in the example.
Fig. 3 is the transmission electron microscope picture of the SiO 2 mesoporous materials of the multilayer sleeve structure that obtains in the example.
Concrete embodiment:
Embodiment 1
Earlier with 0.32g (1mmol) C
14(n=14 B is Na to-L-AlaS
+) be dissolved in 22g (1.22mol) deionized water, at room temperature stir and make its dissolving; Add 12g (0.1mmol) 0.01M hydrochloric acid soln, at room temperature stirred 20-30 minute; Putting into 0 ℃ stirred 10-15 hour down, the basic silane that adds the band amido helps structure directing agent (3-aminopropyl triethoxysilane) 2.0mmol, organosilane (tetraethoxy) 7mmol being added stirs in the mixture again left standstill 1-2 days under back 0 ℃, through centrifugation, deionized water wash, 30 ℃ of dryings, extracting, obtain having the silicon-dioxide hollow tubular mesoporous material of multilayer sleeve structure, the hollow tubular length of material is 3-10 μ m, and outside diameter is 150-200nm, and interior diameter is 50-60nm, the mesoporous aperture of this material is about 3.6nm, and pore volume is about 600mm
3g
-1, specific surface area is 507m
2g
-1Fig. 2 is the sem photograph of this SiO 2 mesoporous materials, and its pattern is the hollow tubular material with multilayer sleeve structure as seen from the figure; Fig. 3 is the transmission electron microscope picture of this mesoporous material, and uniform distribution is mesoporous on this as seen from the figure material wall.
Embodiment 2
Earlier with 0.32g (1mmol) C
14(n=16 B is K to-D-AlaS
+) be dissolved in 22g (1.22mol) deionized water, at room temperature stir and make its dissolving; Add 12g (0.1mmol) 0.01M hydrochloric acid soln, at room temperature stirred 20-30 minute; Putting into 0 ℃ stirred 10-15 hour down, the basic silane that adds the band amido helps structure directing agent (3-aminopropyl triethoxysilane) 2.0mmol, organosilane (tetraethoxy) 7mmol being added stirs in the mixture again left standstill 1-2 days under back 0 ℃, through centrifugation, deionized water wash, 30 ℃ of dryings, extracting, obtain having the silicon-dioxide hollow tubular mesoporous material of multilayer sleeve structure, the hollow tubular length of material is 3-10 μ m, and outside diameter is 150-200nm, and interior diameter is 50-60nm, the mesoporous aperture of this material is about 3.6nm, and pore volume is about 600mm
3g
-1, specific surface area is 507m
2g
-1
Embodiment 3
Earlier with 0.32g (1mmol) C
14(n=14 B is NH to-L-AlaS
4 +) be dissolved in 9g (0.5mol) deionized water, at room temperature stir and make its dissolving; Add 24g (0.2mmol) 0.01M bromic acid solution, at room temperature stirred 20-30 minute; Putting into 0 ℃ stirred 10-15 hour down, the basic silane that adds the band amido helps structure directing agent (3-aminopropyl trimethoxysilane) 2.5mmol, organosilane (methyl silicate) 5mmol being added stirs in the mixture again left standstill 1-2 days under back 0 ℃, through centrifugation, deionized water wash, 30 ℃ of dryings, extracting, obtain having the mesoporous SiO 2 hollow tubular material of multilayer sleeve structure, the hollow tubular length of material is 3-10 μ m, and outside diameter is 150-200nm, and interior diameter is 50-60nm, the mesoporous aperture of this material is about 3.6nm, and pore volume is about 600mm
3g
-1, specific surface area is 600m
2g
-1
Embodiment 4
Earlier with 0.32g (1mmol) C
14(n=16 B is Na to-L-AlaS
+) be dissolved in 72g (4mol) deionized water, at room temperature stir and make its dissolving; Add 12g (0.1mmol) 0.01M salpeter solution, at room temperature stirred 20-30 minute; Putting into 0 ℃ stirred 10-15 hour down, the basic silane that adds the band amido helps structure directing agent (3-aminopropyl trimethoxysilane) 2.0mmol, organosilane (methyl silicate) 10mmol being added stirs in the mixture again left standstill 1-2 days under back 0 ℃, through centrifugation, deionized water wash, 30 ℃ of dryings, extracting, obtain having the silicon-dioxide hollow tubular mesoporous material of multilayer sleeve structure, the hollow tubular length of material is 3-10 μ m, and outside diameter is 150-200nm, and interior diameter is 50-60nm, the mesoporous aperture of this material is about 3.6nm, and pore volume is about 600mm
3g
-1, specific surface area is 507m
2g
-1
Embodiment 5
Earlier with 0.29g (1mmol) C
14-L-AlaA (n=14) is dissolved in 10g (0.56mol) deionized water, add 8g (1mmol) 0.1M sodium hydroxide solution again, at room temperature stir and make its dissolving, add 10g (0.1mmol) 0.01M hydrochloric acid soln again, stirred 20-30 minute, putting into 0 ℃ again stirred 10-15 hour down, the basic silane that adds the band amido helps structure directing agent (3-aminopropyl triethoxysilane) 2.0mmol, organosilane (tetraethoxy) 7mmol being added stirs in the mixture again left standstill 1-2 days under back 0 ℃, through centrifugation, and deionized water wash, 30 ℃ of dryings, extracting obtains having the mesoporous SiO 2 hollow tubular material of multilayer sleeve structure, and the hollow tubular length of material is 3-10 μ m, outside diameter is 150-200nm, interior diameter is 50-60nm, and the mesoporous aperture of this material is 3.6nm, and pore volume is 600mm
3g
-1, specific surface area is 510m
2g
-1
Embodiment 6
Earlier with 0.29g (1mmol) C
14-L-AlaA (n=14) is dissolved in 9g (0.50mol) deionized water, add 8g (1mmol) 0.1M potassium hydroxide solution again, at room temperature stir and make its dissolving, add 20g (0.2mmol) 0.01M hydrochloric acid soln again, stirred 20-30 minute, putting into 0 ℃ again stirred 10-15 hour down, the basic silane that adds the band amido helps structure directing agent (3-aminopropyl triethoxysilane) 2.5mmol, organosilane (tetraethoxy) 5mmol being added stirs in the mixture again left standstill 1-2 days under back 0 ℃, through centrifugation, and deionized water wash, 30 ℃ of dryings, extracting obtains having the silicon-dioxide hollow tubular mesoporous material of multilayer sleeve structure, and the hollow tubular length of material is 3-10 μ m, outside diameter is 150-200nm, interior diameter is 50-60nm, and the mesoporous aperture of this material is 3.6nm, and pore volume is 600mm
3g
-1, specific surface area is 550m
2g
-1
Embodiment 7
Earlier with 0.29g (1mmol) C
14-L-AlaA (n=16) is dissolved in 72g (4mol) deionized water, add 11.2g (1mmol) 0.1M sodium hydroxide solution again, at room temperature stir and make its dissolving, add 10g (0.1mmol) 0.01M bromic acid solution again, stirred 20-30 minute, putting into 0 ℃ again stirred 10-15 hour down, the basic silane that adds the band amido helps structure directing agent (3-aminopropyl trimethoxysilane) 2.0mmol, organosilane (methyl silicate) 10mmol being added stirs in the mixture again left standstill 1-2 days under back 0 ℃, through centrifugation, and deionized water wash, 30 ℃ of dryings, extracting obtains having the hollow tubular SiO 2 mesoporous materials of multilayer sleeve structure, and the hollow tubular length of material is 3-10 μ m, outside diameter is 150-200nm, interior diameter is 50-60nm, and the mesoporous aperture of this material is 3.6nm, and pore volume is 600mm
3g
-1, specific surface area is 530m
2g
-1
Embodiment 8
Earlier with 0.29g (1mmol) C
14-D-AlaA (n=14) is dissolved in 10g (0.56mol) deionized water, add 8g (1mmol) 0.1M sodium hydroxide solution again, at room temperature stir and make its dissolving, add 5g (0.05mmol) 0.01M sulphuric acid soln again, stirred 20-30 minute, putting into 0 ℃ again stirred 10-15 hour down, the basic silane that adds the band amido helps structure directing agent (3-aminopropyl triethoxysilane) 2.5mmol, organosilane (as tetraethoxy) 10mmol being added stirs in the mixture again left standstill 1-2 days under back 0 ℃, through centrifugation, and deionized water wash, 30 ℃ of dryings, extracting obtains having the mesoporous SiO 2 hollow tubular material of multilayer sleeve structure, and the hollow tubular length of material is 3-10 μ m, outside diameter is 150-200nm, interior diameter is 50-60nm, and the mesoporous aperture of this material is 3.6nm, and pore volume is 600mm
3g
-1, specific surface area is 580m
2g
-1
Claims (10)
1. SiO 2 mesoporous materials, for having the mesoporous silicon oxide hollow tubular material of multilayer sleeve structure, wherein, the length of hollow tubular material is 3-10 μ m, and outside diameter is 150-200nm, and interior diameter is 50-60nm, and specific surface area is 500-600m
2g
-1, uniform distribution amido on the mesoporous wall.
2. SiO 2 mesoporous materials according to claim 1 is characterized in that the mesoporous aperture of described mesoporous material is 3-4nm, and pore volume is 300-600mm
3g
-1
3. the preparation method of SiO 2 mesoporous materials as claimed in claim 1 or 2, be that salt with the acid of chirality anion surfactant or chirality anion surfactant is as the main structure directed agents, in the presence of alkali or acid, with the basic silane of band amido for helping structure directing agent, and with the organosilane for the reaction acquisition of silicon source.
4. as the preparation method of SiO 2 mesoporous materials as described in the claim 3, be selected from following arbitrary:
Method one comprises the following steps:
1) preparation of colloidal sol:
The aqueous solution of acid, deionized water and the alkali of chirality anion surfactant is at room temperature mixed preparation colloidal sol;
2) colloidal sol that step 1 is obtained stirred 10-15 hour under-1～1 ℃, and the basic silane that adds the band amido earlier helps structure directing agent, adds organosilane again, leaves standstill 1-2 days under-1～1 ℃ after mixing;
3) obtain to have the mesoporous silicon oxide hollow tubular material of multilayer sleeve structure through separation, washing, drying and suction filtration;
Method two comprises the following steps:
1) preparation of colloidal sol:
Salt, deionized water and the inorganic aqueous acid of chirality anion surfactant are at room temperature mixed preparation colloidal sol;
2) colloidal sol with step 1 acquisition stirred 10-15 hour down at-1～1 ℃, and the basic silane that adds the band amido helps structure directing agent and organosilane, leaves standstill 1-2 days under-1～1 ℃ after mixing;
3) obtain to have the mesoporous silicon oxide hollow tubular material of multilayer sleeve structure through separation, washing, drying and suction filtration.
5. as the preparation method of SiO 2 mesoporous materials as described in the claim 4, it is characterized in that:
In the described method one, the acid of described chirality anion surfactant is N alkyl acyl for-L-L-Ala or N alkyl acyl for-D-L-Ala, meets following structural:
Wherein, R
1Be C
nH
2n+1, n=14 or 16; A is COO
-
In the described method two, the salt of described chirality anion surfactant is N-alkyl acyl for-L-L-Ala salt or N-alkyl acyl for-D-L-Ala salt, meets following structural:
Wherein, R
1Be C
nH
2n+1, n=14 or 16; A is COO
-; B is Na
+, K
+, NH
4 +
6. as the preparation method of SiO 2 mesoporous materials as described in the claim 4, it is characterized in that: in the described method one, the acid of described chirality anion surfactant be selected from N-tetradecyl acyl for-L-L-Ala, N-hexadecyl acyl for-L-L-Ala, N-tetradecyl acyl for-D-L-Ala and N-hexadecyl acyl for-D-L-Ala; In the described method two, the salt of described chirality anion surfactant is selected from N-tetradecyl acyl and replaces-L-L-Ala sylvite, N-hexadecyl acyl replaces-L-L-Ala sylvite, N-tetradecyl acyl replaces-L-L-Ala sodium salt, N-hexadecyl acyl replaces-L-L-Ala sodium salt, N-tetradecyl acyl replaces-L-L-Ala ammonium salt, N-hexadecyl acyl replaces-L-L-Ala ammonium salt, N-tetradecyl acyl replaces-D-L-Ala sylvite, N-hexadecyl acyl replaces-D-L-Ala sylvite, N-tetradecyl acyl replaces-D-L-Ala sodium salt, N-hexadecyl acyl replaces-D-L-Ala sodium salt, N-tetradecyl acyl for-D-L-Ala ammonium salt and N-hexadecyl acyl for-D-L-Ala ammonium salt.
7. as the preparation method of SiO 2 mesoporous materials as described in the claim 4, it is characterized in that:
In the described method one, the acid of described chirality anion surfactant: deionized water: alkali: the basic silane of band amido: the mol ratio of organosilane is 1: 500-4000: 0.8-0.9: 2.0-2.5: 5-10;
In the described method two, the salt of described chirality anion surfactant: deionized water: mineral acid: the basic silane of band amido: the mol ratio of organosilane is 1: 500-4000: 0.1-0.2: 2.0-2.5: 5-10.
8. as the preparation method of SiO 2 mesoporous materials as described in the claim 4, it is characterized in that in the described method one, described alkali is sodium hydroxide, potassium hydroxide or short chain small molecule amine; In the described method two, described mineral acid is sulfuric acid, hydrochloric acid, Hydrogen bromide or nitric acid.
As claim 3-8 arbitrary as described in the preparation method of SiO 2 mesoporous materials, it is characterized in that, the basic silane of described band amido, its structural formula meets following formula:
(R
1O)
3Si—?R—NH
2
Wherein, R
1Be C
1-C
4Straight chain, branched chain alkyl or hydrogen atom; R is C
1-C
4Straight chain or branched chain alkyl;
Described organosilane meets following formula:
(R
1O)m——Si——R
n
Wherein, the integer of m=2-4, R
1Be C
1-C
4Straight chain, branched chain alkyl or hydrogen atom; The integer of n=0-2, R are C
1-C
4Straight chain or branched chain alkyl, m+n=4.
10. as the preparation method of SiO 2 mesoporous materials as described in the claim 8, it is characterized in that the basic silane of described band amido is selected from 3-aminopropyl trimethoxysilane, 3-aminopropyl triethoxysilane and 4-ammonia butyl trimethoxy silane; Described organosilane is selected from tetramethoxy-silicane, tetraethoxysilane, tetrapropoxysilane, tetraisopropoxysilan, four butoxy silanes, dimethoxy dimethylsilane, trimethoxymethylsila,e and dimethoxy di-isopropyl silane.
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Cited By (5)
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| CN103224239A (en) * | 2013-04-08 | 2013-07-31 | 天津大学 | Chiral mesoporous silica nano-rod and preparation method thereof |
| CN103341171A (en) * | 2013-07-12 | 2013-10-09 | 四川大学 | Preparation method of dissolution type silicon dioxide xerogel drug sustained-release material |
| CN104530652A (en) * | 2014-12-25 | 2015-04-22 | 华中科技大学 | Epoxy resin-silicon dioxide hollow tube composite material and preparation method thereof |
| US20150140420A1 (en) * | 2012-05-03 | 2015-05-21 | Iucf-Hyu (Inustry-University Cooperation Foundatio Hanyang University | Method for manufacturing carbon-sulfur composite, carbon-sulfur composite manufactured thereby, and electrochemical device including the same |
| CN113562737A (en) * | 2021-07-29 | 2021-10-29 | 沈阳药科大学 | Mesoporous silica nanoparticle with adjustable chiral structure and preparation method and application thereof |
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| US20150140420A1 (en) * | 2012-05-03 | 2015-05-21 | Iucf-Hyu (Inustry-University Cooperation Foundatio Hanyang University | Method for manufacturing carbon-sulfur composite, carbon-sulfur composite manufactured thereby, and electrochemical device including the same |
| CN103224239A (en) * | 2013-04-08 | 2013-07-31 | 天津大学 | Chiral mesoporous silica nano-rod and preparation method thereof |
| CN103341171A (en) * | 2013-07-12 | 2013-10-09 | 四川大学 | Preparation method of dissolution type silicon dioxide xerogel drug sustained-release material |
| CN104530652A (en) * | 2014-12-25 | 2015-04-22 | 华中科技大学 | Epoxy resin-silicon dioxide hollow tube composite material and preparation method thereof |
| CN104530652B (en) * | 2014-12-25 | 2017-02-22 | 华中科技大学 | Epoxy resin-silicon dioxide hollow tube composite material and preparation method thereof |
| CN113562737A (en) * | 2021-07-29 | 2021-10-29 | 沈阳药科大学 | Mesoporous silica nanoparticle with adjustable chiral structure and preparation method and application thereof |
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