CN103043676B - A kind of mesoporous material - Google Patents
A kind of mesoporous material Download PDFInfo
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- CN103043676B CN103043676B CN201210551526.XA CN201210551526A CN103043676B CN 103043676 B CN103043676 B CN 103043676B CN 201210551526 A CN201210551526 A CN 201210551526A CN 103043676 B CN103043676 B CN 103043676B
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- mesoporous material
- carbon source
- added dropwise
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- 239000013335 mesoporous material Substances 0.000 title claims abstract description 21
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 13
- JJTUDXZGHPGLLC-UHFFFAOYSA-N lactide Chemical compound CC1OC(=O)C(C)OC1=O JJTUDXZGHPGLLC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 21
- 239000007787 solid Substances 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 238000000137 annealing Methods 0.000 claims description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical group CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 2
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 4
- 150000007513 acids Chemical group 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract description 2
- 238000010189 synthetic method Methods 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 description 4
- JKGITWJSGDFJKO-UHFFFAOYSA-N ethoxy(trihydroxy)silane Chemical class CCO[Si](O)(O)O JKGITWJSGDFJKO-UHFFFAOYSA-N 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 2
- 238000007445 Chromatographic isolation Methods 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses a kind of mesoporous material, carbon matrix precursor (i.e. carbon source) is used as by the use of lactide, ethylene glycol and SBA 15 are mixed jointly, obtain the mesoporous material for possessing stronger acids position, which is easy to get, specific surface area is big, synthetic method is simple, mild condition, and duct order is good, it is excellent to the absorption property of heavy metal as sorbing material.
Description
Technical field
The present invention relates to a kind of preparation of mesoporous material.
Background technology
Mesoporous material is a kind of porous material of aperture between 2~50nm, its specific surface area is big, even aperture distribution.
Have the characteristics that shape selectivity is good, diffusivity is high, adsorption capacity is strong, and also good electric conductivity, mechanical stability and heat
Stability, and most of for chemical reaction inertia, available for adsorb, be catalyzed, the field such as electrochemistry, chromatographic isolation.
Stucky in 1998 etc. makees template using p123 first, has prepared the SBA-15 of two-dimentional hexagonal structure, it has
There are larger aperture, wall thickness and hydrothermal stability.But simple silicon skeleton only contains a small amount of weak acid center, so as to limit it
Using then, other atoms can be introduced, increase acid site quantity and intensity, improve skeleton property, ion-exchange performance, expands
Mesoporous material application range.
The content of the invention
The present invention, as carbon source, using SBA-15 as template, adds ethylene glycol as common acid site, synthesis using lactide
Ordered mesoporous material.
The preparation process of ordered mesoporous material of the present invention is：
1) dissolving of template：5~8 parts of template p123 and 6~9 parts of ethylene glycol are dissolved in concentration as 100~150
In the dilute hydrochloric acid of 1.0~1.5mol/L of part, under the conditions of 30~35 DEG C of constant temperature, 450~500rpm stirs 8~12h.
2) addition of silicon source：10~15 parts of silicon sources are added dropwise under 650~800rpm mixing speeds, after being added dropwise completely, continue
Stir and be warming up to 80 DEG C with the speed of 2 DEG C/min, then stand 12~24h of insulation, obtain solid A.
3) carbon source impregnates：1~1.5 part of carbon source is dissolved in ethanol, is stirred evenly.Then while stirring, while being added dropwise
0.3~0.5 part of concentrated sulfuric acid, then adds the solid A for being ground to 100~160 mesh, continues 5~8h of stirring, after equal solvent volatilization
Mixture, keeps the temperature 6h at 100 DEG C, is then heated rapidly to 130~150 DEG C, keep the temperature 8~10h, obtain solid matter B.
4) high annealing：Solid matter B is opened into dry 12h in 50~80 DEG C of vacuum, then in hydrogen atmosphere high temperature annealing 4
~6h, the then natural cooling in hydrogen atmosphere, up to mesoporous material.
Wherein, silicon source described in step 2) is ethyl orthosilicate, and carbon source described in step 3) is lactide.
Wherein, the mass volume ratio of carbon source and ethanol is 1g: 4mL in the step 3).
The present invention's mixes, is gathered around by the use of lactide as carbon matrix precursor (i.e. carbon source), ethylene glycol and SBA-15 jointly
There is the mesoporous material of stronger acids position, which is easy to get, and specific surface area is big, and synthetic method is simple, mild condition,
Duct order is good, excellent to the absorption property of heavy metal as sorbing material.
Embodiment
With reference to the embodiment technical solution that the present invention will be described in detail, but protection domain is not limited thereto.
A kind of 1 mesoporous material of embodiment
5p123 and 7 part of ethylene glycol is dissolved in dilute hydrochloric acid of the concentration for 100 parts of 1.5mol/L, 35 DEG C of conditions of constant temperature
Under, 500rpm stirrings 8h.
15 parts of ethyl orthosilicates are added dropwise under 800rpm mixing speeds, after being added dropwise completely, continue stirring and with 2 DEG C/min's
Speed is warming up to 80 DEG C, then stands insulation 24h, obtains solid A.
1.5 parts of lactides are dissolved in ethanol, are stirred evenly.Then while stirring, while 0.5 part of concentrated sulfuric acid is added dropwise,
Then the solid A for being ground to 100 mesh is added, continues to stir 6h, obtains mixture after equal solvent volatilization, keep the temperature 6h at 100 DEG C, then
130 DEG C are heated rapidly to, 8h is kept the temperature, obtains solid matter B.
Solid matter B is opened into dry 12h in 50 DEG C of vacuum, then hydrogen atmosphere high temperature anneal 6h, then in hydrogen gas
Natural cooling in atmosphere, up to mesoporous material.
A kind of 2 mesoporous material of embodiment
8 parts p123 and 9 part of ethylene glycol is dissolved in dilute hydrochloric acid of the concentration for 150 parts of 1.0mol/L, 30 DEG C of bars of constant temperature
Under part, 500rpm stirrings 10h.
10 parts of ethyl orthosilicates are added dropwise under 700rpm mixing speeds, after being added dropwise completely, continue stirring and with 2 DEG C/min's
Speed is warming up to 80 DEG C, then stands insulation 20h, obtains solid A.
1 part of lactide is dissolved in ethanol, is stirred evenly.Then while stirring, while 0.3 part of concentrated sulfuric acid is added dropwise, so
The solid A for being ground to 120 mesh is added afterwards, continues 5~8h of stirring, mixture is obtained after equal solvent volatilization, keep the temperature 6h at 100 DEG C, so
After be heated rapidly to 130~150 DEG C, keep the temperature 10h, obtain solid matter B.
Solid matter B is opened into dry 12h in 80 DEG C of vacuum, then hydrogen atmosphere high temperature anneal 4h, then in hydrogen gas
Natural cooling in atmosphere, up to mesoporous material.
A kind of 3 mesoporous material of embodiment
7 parts p123 and 8 part of ethylene glycol is dissolved in dilute hydrochloric acid of the concentration for 120 parts of 1.0~1.5mol/L, constant temperature 32
Under the conditions of DEG C, 500rpm stirrings 12h.
12 parts of ethyl orthosilicates are added dropwise under 800rpm mixing speeds, after being added dropwise completely, continue stirring and with 2 DEG C/min's
Speed is warming up to 80 DEG C, then stands insulation 24h, obtains solid A.
1.2 parts of lactides are dissolved in ethanol, are stirred evenly.Then while stirring, while 0.4 part of concentrated sulfuric acid is added dropwise,
Then the solid A for being ground to 120 mesh is added, continues to stir 8h, obtains mixture after equal solvent volatilization, keep the temperature 6h at 100 DEG C, then
150 DEG C are heated rapidly to, 8h is kept the temperature, obtains solid matter B.
Solid matter B is opened into dry 12h in 80 DEG C of vacuum, then hydrogen atmosphere high temperature anneal 4h, then in hydrogen gas
Natural cooling in atmosphere, up to mesoporous material.
In order to confirm the technique effect of the present invention, the present invention is provided with experimental example, to heretofore described mesoporous material
Quick adsorption effect and saturation absorption to heavy metal is measured, and acquired results are as follows：
The preparation of standard heavy metal solution：With copper nitrate, plumbi nitras powder is dissolved in deionized water, and compound concentration is
The heavy metal solution 250mL of 2mmol/L, it is 6.0 to adjust pH.
Vibrate adsorption experiment：20mL standard heavy metal solutions are respectively pipetted in 4 conical flasks, then respectively add mesoporous material
(this experiment used is to be prepared in example example 1) 20mg, then 25 DEG C of constant temperature oscillations in constant temperature oscillator.
Interpretation of result：Absorption result is measured with infrared visible spectrophotometer, adsorption time is respectively 5min, 10min,
30min, 60min, 120min, 250min (90min or so reaches saturation, is as a result averaged for 4 measure numerical value).
| Adsorbance | 5min | 10min | 30min | 60min | 120min |
| Cu(II) | 8.21mg/g | 16.75mg/g | 27.14mg/g | 33.80mg/g | 39.43mg/g |
| Pb(II) | 10.86mg/g | 23.46mg/g | 34.44mg/g | 45.51mg/g | 48.32mg/g |
Claims (1)
- A kind of 1. preparation method of mesoporous material, it is characterised in that：The preparation method is：1）The dissolving of template：5~8 parts of template p123 and 6~9 parts of ethylene glycol are dissolved in concentration as 100~150 parts In the dilute hydrochloric acid of 1.0~1.5mol/L, under the conditions of 30~35 DEG C of constant temperature, 450~500rpm stirs 8~12h；2）The addition of silicon source：10~15 parts of silicon sources are added dropwise under 650~800rpm mixing speeds, after being added dropwise completely, continue to stir And 80 DEG C are warming up to the speed of 2 DEG C/min, 12~24h of insulation is then stood, obtains solid A, the silicon source is ethyl orthosilicate；3）Carbon source impregnates：1~1.5 part of carbon source is dissolved in ethanol, the mass volume ratio of carbon source and ethanol is 1g：4mL, stirring Uniformly, then while stirring, while 0.3~0.5 part of concentrated sulfuric acid is added dropwise, then addition is ground to the solid A of 100~160 mesh, after 5~8h of continuous stirring, mixture is obtained after equal solvent volatilization, and 6h are kept the temperature at 100 DEG C, is then heated rapidly to 130~150 DEG C, insulation 8 ~10h, obtains solid matter B, and the carbon source is lactide；4）High annealing：Solid matter B is opened into dry 12h in 50~80 DEG C of vacuum, then hydrogen atmosphere high temperature anneal 4~ 6h, the then natural cooling in hydrogen atmosphere, up to mesoporous material.
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| CN201210551526.XA CN103043676B (en) | 2012-12-18 | 2012-12-18 | A kind of mesoporous material |
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| CN103043676B true CN103043676B (en) | 2018-04-24 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102275898A (en) * | 2011-07-18 | 2011-12-14 | 天津神能科技有限公司 | High-thermostability ordered mesoporous carbon material and preparation method thereof |
| CN102284085A (en) * | 2011-08-24 | 2011-12-21 | 华南理工大学 | Preparation method of hexagonal mesoporous silica enhanced polyglycolide-lactide microspherical stent |
| CN102614819A (en) * | 2012-04-17 | 2012-08-01 | 哈尔滨工业大学 | Method for preparing magnetic mesoporous carbon nanometer microspheres with high adsorption property |
-
2012
- 2012-12-18 CN CN201210551526.XA patent/CN103043676B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102275898A (en) * | 2011-07-18 | 2011-12-14 | 天津神能科技有限公司 | High-thermostability ordered mesoporous carbon material and preparation method thereof |
| CN102284085A (en) * | 2011-08-24 | 2011-12-21 | 华南理工大学 | Preparation method of hexagonal mesoporous silica enhanced polyglycolide-lactide microspherical stent |
| CN102614819A (en) * | 2012-04-17 | 2012-08-01 | 哈尔滨工业大学 | Method for preparing magnetic mesoporous carbon nanometer microspheres with high adsorption property |
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Inventor after: Su Jianli Inventor before: Feng Yilin Inventor before: Li Ye Inventor before: Song Fulai Inventor before: Cao Liang |
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