CN101597064A - The preparation method of silicon dioxide mesoporous fiber - Google Patents
The preparation method of silicon dioxide mesoporous fiber Download PDFInfo
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- CN101597064A CN101597064A CNA2009100490086A CN200910049008A CN101597064A CN 101597064 A CN101597064 A CN 101597064A CN A2009100490086 A CNA2009100490086 A CN A2009100490086A CN 200910049008 A CN200910049008 A CN 200910049008A CN 101597064 A CN101597064 A CN 101597064A
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Abstract
A kind of preparation method of silicon dioxide mesoporous fiber of technical field of inorganic material, concrete steps are as follows: DNA is added in the ion exchanged water, stir, DNA is dissolved fully, add acid/alkali, regulate pH 3.0～12.0; Keeping adding the basic silane and the organosilane of band amido or quaternary ammonium salt under the agitation condition, continue to stir 5～30 minutes, 0 ℃～60 ℃ standing and reacting 3～9 days, centrifugal, obtain precipitation, use the ion-exchange water washing, vacuum-drying obtains SiO 2 mesoporous materials; DNA wherein: ion exchanged water: acid/alkali: the basic silane of band amido or quaternary ammonium salt: the mol ratio of organosilane is 1: 5000～20000: x (acid: x=0.01～0.5; Alkali: x=0.05～5): 0.75～3: 10～40.Method of the present invention can be prepared the SiO 2 mesoporous materials with chiral structure, has realized the copy of the chiral structure of DNA.
Description
Technical field
That the present invention relates to is a kind of preparation method's of technical field of inorganic material, particularly a kind of silicon dioxide mesoporous fiber preparation method.
Background technology
Inorganic porous material has big specific surface area and pore volume, adjustable pore structure, adjustable aperture, the surface properties that can modify and the appearance that can control or the like, thereby in separation, catalysis, sensing and as the every field such as template of synthetic other materials very large application potential is arranged all.Inorganic porous material comprises: poromerics, mesoporous material, large pore material and multilevel hole material.When preparation inorganic hole material, adopt the organic formwork method obtaining diversified inorganic nano structure, thereby obtain people's extensive concern.Mann, S etc. have delivered at " Chemistry of Materials " (materials chemistry) 1997 the 9th phase 2300-2310 page or leaf and have been entitled as " Sol-Gel Synthesis of Organized Matter " (sol-gel method is synthesized an organized material) literary composition, have proposed to duplicate thought and some synthetic examples that organic formwork obtains inorganic structure in the literary composition.Shinkai, the National People's Congress such as the S organic formwork method that developed on a large scale, at van Bommel, K.J.C. etc. have done detailed elaboration in " AngewandteChemie International Edition " (German applied chemistry) 2003 42 phase 980-999 pages or leaves being entitled as in " Organic Templates for the Generation of Inorganic Materials " (organic formwork of synthetic inorganic material) literary composition of delivering.As template synthesizing inorganic hole material, both can utilize it unique and various ordered structure (comprising chirality) can obtain multiple biological-inorganic hybrid material again with biomolecules, have very large application potential at life science.And DNA is more extensively paid close attention to as the core element of vital process.But owing to keeping under the pH condition of DNA native conformation, the skeleton phosphate is electronegative, and the organosilane hydrolyzate in the synthesizing mesoporous silicon dioxide process is also electronegative under this pH, and the two can't directly interact, therefore about the work of this respect seldom.
Find through literature search prior art, Numata, people such as M have delivered at " Angewandte ChemieInternational Edition " (German applied chemistry) 2004 43 phase 3279-3283 pages or leaves and have been entitled as " Sol-Gel Reaction Using DNA as a Template:An Attempt TowardTranscription of DNA into Inorganic Materials " (with DNA is the sol gel reaction of template: be the once trial of inorganic materials with dna replication dna) literary composition, mention in the literary composition, utilizing " joint " molecule is positive charge with the DNA surface conversion, has obtained bar-shaped silicon-dioxide in organic phase.But this method is loaded down with trivial details, and can't well copy the chiral structure of DNA, more can't keep the copy that DNA group chirality is arranged; Che, (nature: Materials science) 2003 the 2nd volume 801-805 pages or leaves are delivered is entitled as " A novel anionic surfactant templating route forsynthesizing mesoporous silica with unique structure " (the synthetic mesoporous silicon oxide with unique texture of a kind of novel anion surfactant template) literary composition to S etc. at " Nature Materials ", comment in the literary composition, utilization helps the structure directing method to synthesize the anion surfactant Metaporous silicon dioxide material, to help the structure directing method to be used for DNA is template synthesizing mesoporous silicon dioxide material, not only simple to operate, well duplicated the duplex profile of DNA, can keep simultaneously the copy that the phosphate group of DNA spiral is arranged, obtain novel chirality mesoporous earth silicon material, at chiral catalysis, split, and biological field has the potential using value.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art exists, a kind of preparation method of silicon dioxide mesoporous fiber is provided.Method of the present invention can be prepared the SiO 2 mesoporous materials with chiral structure, has fibrous profile, diameter 20nm～50nm, and the hundreds of nanometers of length have and can realize the copy of the chiral structure of DNA with the pore passage structure of potential of hydrogen modulation to several microns.
The present invention is achieved by the following technical solutions, the present invention includes following steps:
1. DNA is added in the ion exchanged water, stir, DNA is dissolved fully, add acid/alkali, regulate pH 3.0～12.0;
2. keeping adding the basic silane and the organosilane of band amido or quaternary ammonium salt under the agitation condition, continue to stir 5～30 minutes, 0 ℃～60 ℃ standing and reacting 3～9 days, centrifugal, obtain precipitation, use the ion-exchange water washing, vacuum-drying obtains SiO 2 mesoporous materials;
DNA wherein: ion exchanged water: acid/alkali: the basic silane of band amido or quaternary ammonium salt: the mol ratio of organosilane is 1: 5000～20000: x (acid: x=0.01～0.5; Alkali: x=0.05～5): 0.75～3: 10～40.
Described acid is a kind of in hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, Hydrogen bromide, perchloric acid or the organic acid.
Described alkali is a kind of in sodium hydroxide, potassium hydroxide, ammoniacal liquor, methylamine or the ethamine.
The basic silane of described band amido or quaternary amine, its structural formula is shown below:
(R
1O)
3Si---B---NR
2R
3Or (R
1O)
3Si---B---N
+R
2R
3R
4X
-
Wherein, R
1, R
2, R
3And R
4Be C
1-C
4Straight chain, branched chain alkyl or hydrogen atom, B are C
1-C
4Straight chain or branched chain alkane, X
-Be chlorion or bromide anion.
The basic silane of described band amido or quaternary amine is 3-aminopropyl trimethoxysilane, 3-aminopropyl triethoxysilane, 4-ammonia butyl trimethoxy silane; N-trimethoxy propyl silane-N-methylamine, N-trimethoxy propyl silane-N, N-dimethyl amine, N-triethoxy propyl silane-N, N-dipropylamine, N-triethoxy propyl silane-N-butylamine, N-trimethoxy propyl silane-N, N, the N-trimethyl ammonium chloride, or N-trimethoxy propyl silane-N, N, a kind of in the N-tributyl brometo de amonio.
Described organosilane, its structure is shown below:
(R
1O)
m——Si——X
n
Wherein, the integer of m=2～4, the integer of n=0～2, R
1Be C
1-C
4Straight chain, branched chain alkyl or hydrogen atom; X is C
1-C
4Straight chain or branched chain alkyl.
Described organosilane is a kind of in tetramethoxy-silicane, tetraethoxysilane, tetrapropoxysilane, tetraisopropoxysilan, four butoxy silanes, dimethoxy dimethylsilane, trimethoxymethylsila,e or the dimethoxy di-isopropyl silane.
The present invention is template with DNA, for helping structure directing agent, is silica source with the organo-siloxane with the basic silane of band amido or quaternary ammonium salt, the regulator solution potential of hydrogen, and the aggregation extent of control template DNA, thus control pore passage structure.Help the cation quaternary ammonium salt group of structure directing agent (basic silane of band amido or quaternary ammonium salt) or aminoly pass through replacement(metathesis)reaction or neutralization reaction generation electrostatic interaction with DNA skeleton phosphate, organoalkoxysilane part and organosilane copolymerization, the silicon-dioxide wall is advanced in condensation, thereby not only can copy the duplex profile of DNA, also may on wall, stay the cation quaternary ammonium salt group of helical arrangement, the helical arrangement of copy DNA phosphate group.
The present invention is silica source with the organosilane, with accumulative DNA under the different pH values is template, with the basic silane of band amido or quaternary ammonium salt is the SiO 2 mesoporous materials that helps structure directing agent to prepare to have chiral structure, has fibrous profile, diameter 20nm～50nm, the hundreds of nanometers of length are to several microns, and having can be with the pore passage structure of potential of hydrogen modulation, duct, ring-type duct and the foraminous spiral tract etc. that comprise ordered arrangement have been realized the copy of the chiral structure of DNA.
Description of drawings
Fig. 1 is the synthesis mechanism synoptic diagram of silicon dioxide mesoporous fiber;
Fig. 2 is the electromicroscopic photograph of silicon dioxide mesoporous fiber.
Embodiment
Following example will the invention will be further described in conjunction with the accompanying drawings.Present embodiment has provided detailed embodiment and process being to implement under the prerequisite with the technical solution of the present invention, but protection scope of the present invention is not limited to following embodiment.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.
As shown in Figure 1, a represents dna molecular, b represents DNA skeleton phosphate and helps structure directing agent (is example with TMAPS) the positively charged group generation of head electrostatic interaction, making helps structure directing agent and organosilane to accumulate in around the dna molecular, c represents to help structure directing agent and organosilane copolycondensation, the synthetic silica mesoporous fiber, d represents the silicon dioxide mesoporous fiber of roasting removal template, the duct that has internal screw, e represents to remove by extraction the silicon dioxide mesoporous fiber of template, has the duct of internal screw and the group of spiral and arranges.
Embodiment 1
With 0.01g DNA (Sigma, salmon sperm dna Type III) stirring is dissolved in the 10.0g ion exchanged water, add 40 μ l 0.1M HCl solution (this moment, pH value of solution was 5.0～5.5), at 25 ℃, keep under the condition of stirring, add 22.67 μ l massfractions and be N-trimethoxy propyl silane-N of 50%, N, the methanol solution of N-trimethyl ammonium chloride and 106.4 μ l tetraethoxysilanes, add the back and kept stirring reaction 15 minutes, 25 ℃ of standing and reacting 5 days obtain solid matter through centrifugation, use the ion-exchange water washing again, lyophilize one day obtains a kind of silicon dioxide mesoporous fiber; 550 ℃ of roastings 6 hours obtain removing the silicon dioxide mesoporous fiber of organic formwork and functional group.
A among Fig. 2
1Be the stereoscan photograph of this silicon dioxide mesoporous fiber, it shows evenly rule of this silicon dioxide mesoporous fiber, and external diameter is 20nm～30nm, a
2Be the high-resolution-ration transmission electric-lens photo of this silicon dioxide mesoporous fiber, show that this silicon dioxide mesoporous fiber has the pore passage structure of ordered arrangement.
Embodiment 2
With 0.01g DNA (Sigma, salmon sperm dna Type III) stirring is dissolved in (this moment, pH value of solution was 6.5～7.0) in the 10.0g ion exchanged water, 25 ℃, keep under the condition of stirring, add 22.67 μ l massfractions and be N-trimethoxy propyl silane-N of 50%, N, the methanol solution of N-trimethyl ammonium chloride and 106.4 μ l tetraethoxysilanes, add the back and kept stirring reaction 15 minutes, 25 ℃ of standing and reacting 5 days, obtain solid matter through centrifugation, use the ion-exchange water washing again, lyophilize one day obtains a kind of silicon dioxide mesoporous fiber; 550 ℃ of roastings 6 hours obtain removing the silicon dioxide mesoporous fiber of organic formwork and functional group.
B among Fig. 2
1Be the stereoscan photograph of this silicon dioxide mesoporous fiber, it shows evenly rule of this silicon dioxide mesoporous fiber, and external diameter is 30nm～50nm, b
2Be the high-resolution-ration transmission electric-lens photo of this silicon dioxide mesoporous fiber, show that this silicon dioxide mesoporous fiber has tubulose, cyclic pore passage structure.
Embodiment 3
With 0.01g DNA (Sigma, salmon sperm dna Type III) is dissolved in the 10.0g ion exchanged water, add 120 μ l 0.5M NaOH solution (this moment, pH value of solution was 11.5～11.9), at 25 ℃, keep under the condition of stirring, add 22.67 μ l mass fractions and be N-trimethoxy propyl silane-N of 50%, N, the methanol solution of N-trimethyl ammonium chloride and 106.4 μ l tetraethoxysilanes, add the back and kept stirring reaction 15 minutes, 25 ℃ of standing and reacting 5 days obtain solid matter through centrifugation, use the ion-exchange water washing again, lyophilize one day obtains a kind of silicon dioxide mesoporous fiber; 550 ℃ of roastings 6 hours obtain removing the silicon dioxide mesoporous fiber of organic formwork and functional group.
C among Fig. 2
1Be the stereoscan photograph of this silicon dioxide mesoporous fiber, it shows evenly rule of this silicon dioxide mesoporous fiber, and external diameter is 20nm～30nm, c
2Be the high-resolution-ration transmission electric-lens photo of this silicon dioxide mesoporous fiber, show that this silicon dioxide mesoporous fiber has the pore passage structure of spiral.
Embodiment 4
With 0.01g DNA (Sigma, salmon sperm dna Type III) stirring is dissolved in the 10.0g ion exchanged water, add 5 μ l 0.5M KOH solution (this moment, pH value of solution was 8.5～9.5), at 15 ℃, keep under the condition of stirring, add 22.67 μ l massfractions and be N-trimethoxy propyl silane-N of 50%, N, 50% methanol solution of N-trimethylammonium bromide and 111.9 μ l tetraisopropoxysilan, add the back and kept stirring reaction 15 minutes, 15 ℃ of standing and reacting 5 days obtain solid matter through centrifugation, use the ion-exchange water washing again, lyophilize one day, 550 ℃ of roastings 6 hours obtain a kind of silicon dioxide mesoporous fiber.In 0.1M HCl solution, 60 ℃ were stirred 12 hours down, the neutralization back adds quadrol-magnesium chloride mixture solution, and 60 ℃ are continued to stir 12 hours down, obtain the SiO 2 mesoporous materials that template (quaternary ammonium salt group that keeps the duct inwall) removed in extraction behind the centrifuge washing.
Embodiment 5
0.01g DNA (Sigma, salmon sperm dna Type III) stirring is dissolved in the 10.0g ion exchanged water, adds 60 μ l 0.1M CH
3COOH solution (this moment, pH value of solution was 4.5～5.5), 25 ℃, keep under the condition of stirring, add 22.67 μ l massfractions and be N-trimethoxy propyl silane-N of 50%, N, 50% methanol solution of N-trimethyl ammonium chloride and 106.4 μ l tetraethoxysilanes, add the back and kept stirring reaction 15 minutes, 25 ℃ of standing and reacting 5 days obtain solid matter through centrifugation, use the ion-exchange water washing again, lyophilize one day, 550 ℃ of roastings 6 hours obtain a kind of silicon dioxide mesoporous fiber.
Embodiment 6
0.01g DNA (Sigma, salmon sperm dna Type III) stirring is dissolved in the 10.0g ion exchanged water, adds 50 μ l 0.1M H
3PO
4Solution (this moment, pH value of solution was 3.0～4.0), 40 ℃, keep under the condition of stirring, add 6.69 μ l 3-aminopropyl trimethoxysilane and 106.4 μ l tetraethoxysilanes, add the back and kept stirring reaction 15 minutes, 40 ℃ of standing and reacting 3 days obtain solid matter through centrifugation, use the ion-exchange water washing again, lyophilize one day obtains a kind of silicon dioxide mesoporous fiber.In 0.1M HCl solution, 40 ℃ were stirred 12 hours down, and the neutralization back adds quadrol-magnesium chloride mixture solution, and 40 ℃ are continued to stir 12 hours down, obtain the SiO 2 mesoporous materials that template (amino that keeps the duct inwall) is removed in extraction behind the centrifuge washing.
Embodiment 7
0.01g DNA (Sigma, salmon sperm dna Type III) stirring is dissolved in the 10.0g ion exchanged water, adds 60 μ l 0.1M H
2SO
2Solution (this moment, pH value of solution was 3.0～4.0), 30 ℃, keep under the condition of stirring, add 7.13 μ l 4-ammonia butyl trimethoxy silanes and 96.9 μ l tetramethoxy-silicanes, add the back and kept stirring reaction 15 minutes, 30 ℃ of standing and reacting 5 days obtain solid matter through centrifugation, use the ion-exchange water washing again, lyophilize one day obtains a kind of silicon dioxide mesoporous fiber.550 ℃ of roastings 6 hours obtain removing the silicon dioxide mesoporous fiber of organic formwork and functional group.
Claims (7)
1, a kind of preparation method of silicon dioxide mesoporous fiber is characterized in that, comprises the steps:
1. DNA is added in the ion exchanged water, stir, DNA is dissolved fully, add acid/alkali, regulate pH 3.0～12.0;
2. keeping adding the basic silane and the organosilane of band amido or quaternary ammonium salt under the agitation condition, continue to stir 5～30 minutes, 0 ℃～60 ℃ standing and reacting 3～9 days, centrifugal, obtain precipitation, use the ion-exchange water washing, vacuum-drying obtains SiO 2 mesoporous materials;
DNA wherein: ion exchanged water: acid/alkali: the basic silane of band amido or quaternary ammonium salt: the mol ratio of organosilane is 1: 5000～20000: x (acid: x=0.01～0.5; Alkali: x=0.05～5): 0.75～3: 10～40.
2, the preparation method of silicon dioxide mesoporous fiber according to claim 1 is characterized in that, described acid is a kind of in hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, Hydrogen bromide, perchloric acid or the organic acid.
3, the preparation method of silicon dioxide mesoporous fiber according to claim 1 is characterized in that, described alkali is a kind of in sodium hydroxide, potassium hydroxide, ammoniacal liquor, methylamine or the ethamine.
4, the preparation method of silicon dioxide mesoporous fiber according to claim 1 is characterized in that, the basic silane of described band amido or quaternary amine, and its structural formula is shown below:
(R
1O)
3Si-B-NR
2R
3Or (R
1O)
3Si-B-N
+R
2R
3R
4X
-
Wherein, R
1, R
2, R
3And R
4Be C
1-C
4Straight chain, branched chain alkyl or hydrogen atom, B are C
1-C
4Straight chain or branched chain alkane, X
-Be chlorion or bromide anion.
5, the preparation method of silicon dioxide mesoporous fiber according to claim 1 is characterized in that, the basic silane of described band amido or quaternary amine is 3-aminopropyl trimethoxysilane, 3-aminopropyl triethoxysilane, 4-ammonia butyl trimethoxy silane; N-trimethoxy propyl silane-N-methylamine, N-trimethoxy propyl silane-N, N-dimethyl amine, N-triethoxy propyl silane-N, N-dipropylamine, N-triethoxy propyl silane-N-butylamine, N-trimethoxy propyl silane-N, N, N-trimethyl ammonium chloride, or N-trimethoxy propyl silane-N, N, a kind of in the N-tributyl brometo de amonio.
6, the preparation method of silicon dioxide mesoporous fiber according to claim 1 is characterized in that, described organosilane, and its structure is shown below:
(R
1O)
m-Si-X
n
Wherein, the integer of m=2～4, the integer of n=0～2, R
1Be C
1-C
4Straight chain, branched chain alkyl or hydrogen atom; X is C
1-C
4Straight chain or branched chain alkyl.
7, the preparation method of silicon dioxide mesoporous fiber according to claim 1, it is characterized in that described organosilane is a kind of in tetramethoxy-silicane, tetraethoxysilane, tetrapropoxysilane, tetraisopropoxysilan, four butoxy silanes, dimethoxy dimethylsilane, trimethoxymethylsila,e or the dimethoxy di-isopropyl silane.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108873602A (en) * | 2018-06-29 | 2018-11-23 | 厦门大学 | A method of the production mask plate based on DNA paper folding nanostructure |
| CN109031750A (en) * | 2018-08-22 | 2018-12-18 | 苏州美嘉写智能显示科技有限公司 | A kind of white light writing, reflection enhancement type liquid crystal board and preparation method thereof |
| CN110171833A (en) * | 2019-05-27 | 2019-08-27 | 苏州大学 | A kind of silica nano fibrous base gel composite electrolyte and preparation method thereof |
| CN110713192A (en) * | 2019-11-28 | 2020-01-21 | 常州北化澳联环保科技有限公司 | Preparation method of spherical silicon dioxide nanoparticle slurry |
| CN111777075A (en) * | 2020-08-04 | 2020-10-16 | 河南科技学院 | Preparation method and application of amino-functionalized hierarchical pore structure silicon dioxide |
-
2009
- 2009-04-09 CN CNA2009100490086A patent/CN101597064A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108873602A (en) * | 2018-06-29 | 2018-11-23 | 厦门大学 | A method of the production mask plate based on DNA paper folding nanostructure |
| CN109031750A (en) * | 2018-08-22 | 2018-12-18 | 苏州美嘉写智能显示科技有限公司 | A kind of white light writing, reflection enhancement type liquid crystal board and preparation method thereof |
| CN110171833A (en) * | 2019-05-27 | 2019-08-27 | 苏州大学 | A kind of silica nano fibrous base gel composite electrolyte and preparation method thereof |
| CN110713192A (en) * | 2019-11-28 | 2020-01-21 | 常州北化澳联环保科技有限公司 | Preparation method of spherical silicon dioxide nanoparticle slurry |
| CN111777075A (en) * | 2020-08-04 | 2020-10-16 | 河南科技学院 | Preparation method and application of amino-functionalized hierarchical pore structure silicon dioxide |
| CN111777075B (en) * | 2020-08-04 | 2021-05-07 | 河南工业大学 | Preparation method and application of amino-functionalized hierarchical pore structure silicon dioxide |
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Open date: 20091209 |