CN104140090A - Preparation method of hydrophilic ordered mesopore carbon material - Google Patents
Preparation method of hydrophilic ordered mesopore carbon material Download PDFInfo
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- CN104140090A CN104140090A CN201410376195.XA CN201410376195A CN104140090A CN 104140090 A CN104140090 A CN 104140090A CN 201410376195 A CN201410376195 A CN 201410376195A CN 104140090 A CN104140090 A CN 104140090A
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- carbon material
- tsc
- sba
- mesoporous carbon
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 102100021935 C-C motif chemokine 26 Human genes 0.000 claims abstract description 24
- 101000897493 Homo sapiens C-C motif chemokine 26 Proteins 0.000 claims abstract description 24
- 239000002808 molecular sieve Substances 0.000 claims abstract description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 10
- 238000005119 centrifugation Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000013335 mesoporous material Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- 238000009736 wetting Methods 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- -1 polyethylene Polymers 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 230000010148 water-pollination Effects 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 235000011167 hydrochloric acid Nutrition 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000004375 physisorption Methods 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 230000003068 static effect Effects 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a preparation method of a hydrophilic ordered mesopore carbon material TSC-1. An SBA-15 mesoporous molecular sieve is used as a mother template, and P123 copolymer template agents in the mother template are carbonized under high temperature to generate the ordered mesopore carbon material TSC-1. The ordered mesopore carbon material TSC-1 has the advantages of being good in hydrophily, easy to adjust in diameter compared with a traditional ordered mesopore carbon material, and has wide application prospects in the field of catalysis, energy, environment protection and the like.
Description
Technical field
The invention belongs to chemical technology and field of environment protection, be specifically related to the preparation method of a kind of hydrophilic ordered mesoporous carbon material TSC-1.
Background technology
In recent years, due to the progress of chemical synthesising technology, a large amount of investigators have been developed the ordered mesoporous carbon material of various structures, as CMK series and FDU series etc.Mesoporous carbon material has good chemical stability and thermostability, shows good application prospect at numerous areas such as catalyst support material, energy storage material and sorbing materials.For example CMK-3 can mounted mass mark up to 50% platinum, and still can keep its 2.5 nm compared with small particle size, high platinum carrying capacity makes this material have very high oxygen reduction reactive behavior.In addition, metal active species have higher dispersiveness in CMK-3 than in general porous charcoal duct, make it be expected to become excellent fuel cell electrode material.
But production cost is too high, processing condition are complicated is the two large problems that current ordered mesoporous carbon scale operation still faces.In addition, the performance that traditional ordered mesoporous carbon material wetting ability is not good while greatly having affected it as sorbing material and support of the catalyst yet.Therefore, in the urgent need to develop the manufacture of a kind of novel method all having superiority for ordered mesoporous carbon material in technical difficulty, cost and performance.
Summary of the invention
The problems such as the production cost that exists for traditional ordered mesoporous carbon material is high, complex process, wetting ability are not good, the invention provides a kind of method that technical difficulty is low, cost is controlled and prepare ordered mesoporous carbon material, and its wetting ability improves significantly, in the time that it uses as support of the catalyst, can flood active specy contact fully, make its dispersion more even, be more conducive to the raising of catalyst performance.
The technological line that the present invention adopts is to synthesize first according to actual needs the SBA-15 mesoporous silicon material with target aperture, taking SBA-15 as template, under proper temperature condition, by the inner P123 high-molecular copolymer charing of its duct, obtain TSC-1 ordered mesoporous carbon material finally by alkali lye dissolving SBA-15 template, centrifugation.
The present invention is a kind of preparation method that can modulation aperture ordered mesoporous carbon material, it is characterized in that having following preparation process and step.
A. target aperture SBA-15 mesoporous silica molecular sieve is synthetic: with polyethylene glycol-propylene glycol-polyoxyethylene glycol triblock polymer, (P123, molecular formula is H (OCH2-CH2-)
x[OCH (CH3) CH2-]
y(OCH2CH2-)
zoH, the molar ratio of EO: PO: EO is 20: 70: 20, molecular-weight average is 5800) be template, taking tetraethoxy or water glass as silicon source, synthetic SBA-15 molecular sieve under strong acidic condition, mole the consisting of of reactant: P123: SiO
2: HCl: H
2o=1～2: 40～60: 300～500: 7000～10000.
B. use SBA-15 as caster, its inner P123 multipolymer template is heated to 600～900 DEG C of charings under inert atmosphere, 2.5～5 DEG C/min of temperature rise rate, and keep 3-4 hour, inert atmosphere is N
2or in Ar any.
C. above-mentioned SBA-15/TSC-1 mixture is added in the NaOH solution of 2～4 mol/L, heat and stir after 4～6 hours, obtain TSC-1 ordered mesoporous carbon material finally by 4000～5000 rpm centrifugation 15 min.
The present invention is simple, realized the synthetic of hydrophilic ordered mesoporous carbon material TSC-1, and its aperture is controlled, and at pollutent absorption, catalysis and novel material etc., field is bright has a good application prospect.
embodiment.
Embodiment 1
4 nm aperture TSC-1 ordered mesoporous carbon materials are prepared as follows:
60 mL concentrated hydrochloric acids are dissolved in 312 mL deionized waters to 313 K constant temperature water baths.Then add 15 g P123, use magnetic stirrer constant temperature to stir 4 h, after add TEOS 22.5 g, then constant temperature stirs 24 h.Then mixture is transferred in water heating kettle, after 343 K static crystallization 12 h, filtered to obtain white solid, 393 K are dried.
The SBA-15 mesoporous material that contains P123 template is heated to 750 DEG C of charings under Ar atmosphere, 2.5 DEG C/min of temperature rise rate, and keep 4 hours.Subsequently above-mentioned SBA-15/TSC-1 mixture is added in the NaOH solution of 4 mol/L, heat and stir after 4.5 hours, finally by 4000-5000 rpm centrifugation, 15 min obtain TSC-1 ordered mesoporous carbon material.Confirm that through little angle XRD and nitrogen physisorption sign its pore size is 4 nm.
Embodiment 2
6 nm aperture TSC-1 ordered mesoporous carbon materials are prepared as follows:
60 mL concentrated hydrochloric acids are dissolved in 312 mL deionized waters to 313 K constant temperature water baths.Then add 15 g P123, use magnetic stirrer constant temperature to stir 4 h, after add TEOS 22.5 g, then constant temperature stirs 24 h.Then mixture is transferred in water heating kettle, after 368 K static crystallization 12 h, filtered to obtain white solid, 393 K are dried.
The SBA-15 mesoporous material that contains P123 template is heated to 750 DEG C of charings under Ar atmosphere, 2.5 DEG C/min of temperature rise rate, and keep 4 hours.Subsequently above-mentioned SBA-15/TSC-1 mixture is added in the NaOH solution of 4 mol/L, heat and stir after 4.5 hours, finally by 4000-5000 rpm centrifugation, 15 min obtain TSC-1 ordered mesoporous carbon material.Confirm that through little angle XRD and nitrogen physisorption sign its pore size is 6 nm.
Embodiment 3
10nm aperture TSC-1 ordered mesoporous carbon material is prepared as follows:
60 mL concentrated hydrochloric acids are dissolved in 312 mL deionized waters to 333 K constant temperature water baths.Then add 15 g P123, use magnetic stirrer constant temperature to stir 4 h, after add TEOS 22.5 g, then constant temperature stirs 24 h.Then mixture is transferred in water heating kettle, after 378 K static crystallization 12 h, filtered to obtain white solid, 393 K are dried.
The SBA-15 mesoporous material that contains P123 template is heated to 800 DEG C of charings under Ar atmosphere, 5 DEG C/min of temperature rise rate, and keep 4 hours.Subsequently above-mentioned SBA-15/TSC-1 mixture is added in the NaOH solution of 4 mol/L, heat and stir after 4.5 hours, finally by 4000-5000 rpm centrifugation, 15 min obtain TSC-1 ordered mesoporous carbon material.Confirm that through little angle XRD and nitrogen physisorption sign its pore size is 10 nm.
Embodiment 4
12nm aperture TSC-1 ordered mesoporous carbon material is prepared as follows:
60 mL concentrated hydrochloric acids are dissolved in 312 mL deionized waters to 333 K constant temperature water baths.Then add 15 g P123, use magnetic stirrer constant temperature to stir 4 h, after add TEOS 22.5 g, then constant temperature stirs 24 h.Then mixture is transferred in water heating kettle, after 398 K static crystallization 12 h, filtered to obtain white solid, 393 K are dried.
The SBA-15 mesoporous material that contains P123 template is heated to 900 DEG C of charings under Ar atmosphere, 5 DEG C/min of temperature rise rate, and keep 4 hours.Subsequently above-mentioned SBA-15/TSC-1 mixture is added in the NaOH solution of 4 mol/L, heat and stir after 4.5 hours, finally by 4000-5000 rpm centrifugation, 15 min obtain TSC-1 ordered mesoporous carbon material.Confirm that through little angle XRD and nitrogen physisorption sign its pore size is 12 nm.
Claims (3)
1. the present invention is a kind of preparation method of hydrophilic ordered mesoporous carbon material, it is characterized in that having following preparation process and step:
A. target aperture SBA-15 mesoporous silica molecular sieve is synthetic: with polyethylene glycol-propylene glycol-polyoxyethylene glycol triblock polymer, (P123, molecular formula is H (OCH2-CH2-)
x[OCH (CH3) CH2-]
y(OCH2CH2-)
zoH, the molar ratio of EO: PO: EO is 20: 70: 20, molecular-weight average is 5800) be template, taking tetraethoxy or water glass as silicon source, synthetic SBA-15 molecular sieve under strong acidic condition;
B. use SBA-15 as caster, its inner P123 multipolymer template is heated to 600～900 DEG C of charings under inert atmosphere, inert atmosphere is N
2or one in Ar;
C. above-mentioned SBA-15/TSC-1 mixture is added in the NaOH solution of certain 2～4 mol/L, heat and stir after 4-6 hour and obtain TSC-1 ordered mesoporous carbon material through centrifugation.
2. method according to claim 1, is characterized in that TSC-1 mesoporous material carbon element content is 70-80%, oxygen element content 20-30%, and oxygen level is higher, and wetting ability is significantly better than traditional mesoporous carbon material.
3. method according to claim 1, is characterized in that TSC-1 has orderly one-dimensional tunnel structure, and aperture can modulation between 4～15 nm, and specific surface is 1200～1500 m
2/ g.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410376195.XA CN104140090B (en) | 2014-08-02 | 2014-08-02 | A kind of preparation method of hydrophilic ordered mesoporous carbon material |
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|---|---|---|---|
| CN201410376195.XA CN104140090B (en) | 2014-08-02 | 2014-08-02 | A kind of preparation method of hydrophilic ordered mesoporous carbon material |
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| CN104140090A true CN104140090A (en) | 2014-11-12 |
| CN104140090B CN104140090B (en) | 2016-08-31 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111498862A (en) * | 2020-04-03 | 2020-08-07 | 三峡大学 | Preparation method and application of spherical SBA-15 mesoporous molecular sieve |
| CN114471494A (en) * | 2022-01-25 | 2022-05-13 | 甘肃中商食品质量检验检测有限公司 | Preparation method and application of functionalized mesoporous carbon nanocomposite |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1807244A (en) * | 2005-12-21 | 2006-07-26 | 大连理工大学 | Multi-stage porous titanium-silicon zeolite preparation method and its uses in catalytic oxidation |
| 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 |
| CN103482596A (en) * | 2012-06-12 | 2014-01-01 | 北京化工大学 | Preparation method and application of ordered mesoporous carbon |
-
2014
- 2014-08-02 CN CN201410376195.XA patent/CN104140090B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1807244A (en) * | 2005-12-21 | 2006-07-26 | 大连理工大学 | Multi-stage porous titanium-silicon zeolite preparation method and its uses in catalytic oxidation |
| 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 |
| CN103482596A (en) * | 2012-06-12 | 2014-01-01 | 北京化工大学 | Preparation method and application of ordered mesoporous carbon |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111498862A (en) * | 2020-04-03 | 2020-08-07 | 三峡大学 | Preparation method and application of spherical SBA-15 mesoporous molecular sieve |
| CN114471494A (en) * | 2022-01-25 | 2022-05-13 | 甘肃中商食品质量检验检测有限公司 | Preparation method and application of functionalized mesoporous carbon nanocomposite |
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| CN104140090B (en) | 2016-08-31 |
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Address after: 200438 Shanghai city Yangpu District State Road 1450 Lane 27, room 304 Applicant after: Sun Chao Address before: 102205 Beijing city center Changping District Yangfang Town Street No. 37 Applicant before: Sun Chao |
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Granted publication date: 20160831 |