CN103194438A - Preparation method of mesoporous carbon/silicon composite material - Google Patents
Preparation method of mesoporous carbon/silicon composite material Download PDFInfo
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- CN103194438A CN103194438A CN2013101364975A CN201310136497A CN103194438A CN 103194438 A CN103194438 A CN 103194438A CN 2013101364975 A CN2013101364975 A CN 2013101364975A CN 201310136497 A CN201310136497 A CN 201310136497A CN 103194438 A CN103194438 A CN 103194438A
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Abstract
The invention relates to a preparation method of a mesoporous carbon/silicon composite material, and belongs to the field of nano materials. The method comprises the following steps of: dissolving fluronic F127 in a mixed solution formed by ethanol and water at the temperature of 20 to 50 DEG C; then adding resorcinol and ethyl orthosilicate, enabling the concentration of hydrogen chloride (HCl) in the solution to be 0.5M to 2M by adding hydrochloric acid, and adding formaldehyde; enabling the mol ratio of F127, ethanol, water, resorcinol, ethyl orthosilicate and formaldehyde in the reaction system to be (0.01-0.03):20:(20-50):(1-4):(0.5-2):(1-5); and pouring the solution into a culture dish to be aged, enabling a sample to be layered, pouring the upper layer solution of the layered sample, thermally polymerizing the lower viscous system in a baking oven for 12 to 24 hours at the temperature of 100 DEG C to 160 DEG C, then roasting for 1 to 5 hours at the temperature of 600 DEG C to 950 DEG C, and naturally cooling to obtain a sample. The preparation method is simple in process, convenient to operate and strong in repetition.
Description
Technical field
The invention belongs to field of nanometer material technology, the preparation method of a kind of mesoporous carbon/silicon composite of specific design.
Background technology
Meso-porous carbon material is because its bigger specific surface area and pore volume, adjustable aperture structure, higher electroconductibility, physical strength and chemical stability, at N,O-Diacetylmuramidase, cytochrome c, biological enzyme molecule immobilization aspects such as lipase obtain to use widely. the preparation of meso-porous nano matrix material, not only can enrich the kind of mesoporous material, and with respect to the mesoporous material of single-element, can improve its performance, effectively increasing its using value. mesoporous carbon/silicon composite is a kind of important meso-porous nano matrix material, the adding of silicon components in the mesoporous carbon system, can increase the quantity of mesoporous wall surface unsaturated group, improve the modifiability of mesoporous material, and then the modification by organic group causes the increase of enzyme molecule fixed efficiency and immobilization intensity in mesoporous material. in addition, silicon components in the mesoporous system can also improve the stability of single meso-porous carbon material, avoid its skeleton in roasting and use to shrink serious, easily cave in, shortcomings such as the aperture is little improve its use range and number of times in the enzyme fixed catalyst process.
Summary of the invention
The object of the present invention is to provide the preparation method of simple, the easy to operate and repeated strong mesoporous carbon/silicon composite of a kind of preparation technology.
The preparation method of mesoporous carbon/silicon composite provided by the present invention may further comprise the steps:
A kind of preparation method of mesoporous carbon/silicon composite is characterized in that, may further comprise the steps:
1) F127 is dissolved in 20 ℃ ~ 50 ℃ the mixing solutions of second alcohol and water formation;
2) etc. F127 dissolves fully, adds Resorcinol and tetraethoxy in the mixing solutions of step 1), makes that by adding hydrochloric acid HCl concentration continues to stir 2h between 0.5M ~ 2M in the solution;
3) in step 2) add formaldehyde in the solution that obtains, continue to stir 4h and make to react completely and carry out;
F127 in the reaction system: ethanol: water: Resorcinol: tetraethoxy: the mol ratio of formaldehyde is: 0.01 ~ 0.03:20:20 ~ 50:1 ~ 4:0.5 ~ 2:1 ~ 5;
4) solution that step 3) is obtained is poured into ageing in the culture dish, makes the sample layering;
5) layering sample upper solution in the step 4) is outwelled, again with lower floor's thickness system thermopolymerization 12 ~ 24h in 100 ℃ ~ 160 ℃ baking oven;
6) with gained sample in the step 5) at 600 ℃ ~ 950 ℃ roasting 1 ~ 5h of inert atmosphere, gained sample in cooling back is mesoporous carbon/silicon composite naturally.
F127 is triblock copolymer tensio-active agent PEO
106PPO
70PEO
106.
Gained mesoporous carbon/silicon materials have worm meso-porous duct, and its nitrogen adsorption desorption isotherm is the IV thermoisopleth, illustrate that it is meso-hole structure.
Description of drawings:
The TEM of gained mesoporous carbon/silicon composite figure among Fig. 1 embodiment 2
The TEM of gained mesoporous carbon/silicon composite figure among Fig. 2 embodiment 3
The TEM of gained mesoporous carbon/silicon composite figure among Fig. 3 embodiment 4
The nitrogen adsorption desorption isotherm figure of gained mesoporous carbon/silicon composite among Fig. 4 embodiment 4
The graph of pore diameter distribution of gained mesoporous carbon/silicon composite among Fig. 5 embodiment 4
The EDS of gained mesoporous carbon/silicon composite can spectrogram among Fig. 6 embodiment 4
Among Fig. 7 embodiment 4 gained mesoporous carbon/silicon composite to the adsorptive capacity of N,O-Diacetylmuramidase with the enzyme concn change curve
Gained mesoporous carbon/silicon composite is to N,O-Diacetylmuramidase adsorptive capacity change curve in time among Fig. 8 embodiment 4
The TEM of gained mesoporous carbon/silicon composite figure among Fig. 9 embodiment 7
The nitrogen adsorption desorption isotherm figure of gained mesoporous carbon/silicon composite among Figure 10 embodiment 7
The graph of pore diameter distribution of gained mesoporous carbon/silicon composite among Figure 11 embodiment 7
Embodiment:
1) 1.26g F127 is dissolved in 20 ℃ the mixing solutions of 11.5ml ethanol and 3.6ml water formation.
2) etc. F127 dissolves fully, adds 1.1g Resorcinol, 1.1ml tetraethoxy in step 1) solution, and HCl concentration is 0.5M. in the hydrochloric acid conditioning solution by adding
3) continue to stir 2h after, in step 2) add 1ml formaldehyde solution in the solution, under this temperature, continue to stir 4h and make to react completely and carry out.
The F127 that adds in the reaction system: ethanol: water: Resorcinol: tetraethoxy: the mol ratio of formaldehyde is: 0.01:20:20:1:0.5:1.
4) stir stop after, solution in the step 3) is poured into ageing makes the sample layering in the culture dish.
5) layering sample upper solution in the step 4) is outwelled, again with lower floor's thickness system 100
oThermopolymerization 12h. in the baking oven of C
6) the roasting 1h. under 600 ℃ of nitrogen atmospheres of gained sample in the step 5) being lowered the temperature naturally afterwards, the gained sample is mesoporous carbon/silicon composite.
Gained mesoporous carbon/silicon materials have worm meso-porous duct, and its nitrogen adsorption desorption isotherm is the IV thermoisopleth, illustrate that it is meso-hole structure, and the most probable aperture is that 7.6nm. BET specific surface area is 566.5m
2/ g, pore volume are 0.54cm
3/ g.
1) F127, ethanol, water add-on are with embodiment 1, and just the temperature of solution is adjusted into 30 ℃.
2) with embodiment 1, but adding hydrochloric acid conditioned reaction system HCl concentration is 1M.
3) other steps are with embodiment 1.
Gained mesoporous carbon/silicon materials have worm meso-porous duct, measure through the nitrogen adsorption desorption, and embodiment 2 gained material B ET specific surface areas are 559.1m
2/ g, pore volume are 0.56cm
3/ g, the most probable aperture is 9.4nm.
1) 2.5g F127 is dissolved in 30 ℃ the mixing solutions of 12ml ethanol and 8.9ml water formation.
2) etc. F127 dissolves fully, adds 2.2g Resorcinol, 2.2ml tetraethoxy in step 1) solution, and HCl concentration is 1M. in the hydrochloric acid conditioning solution by adding
3) continue to stir 2h after, in step 2) add 2.8ml formaldehyde in the solution, continue to stir 4h again and make to react completely and carry out.
F127 in the reaction system: ethanol: water: Resorcinol: tetraethoxy: the mol ratio of formaldehyde is: 0.02:20:20:2:1:10.
4) with embodiment 1.
5) with embodiment 1.
6) the roasting 1h. under 800 ℃ of nitrogen atmospheres of gained sample in the step 5) being lowered the temperature naturally afterwards, the gained sample is mesoporous carbon/silicon composite.
Gained mesoporous carbon/silicon materials have worm meso-porous duct, measure through the nitrogen adsorption desorption, and gained material B ET specific surface area is 529.5m
2/ g, pore volume are 0.46cm
3/ g, to be 7.5nm. be applied to the immobilization of N,O-Diacetylmuramidase with gained mesoporous carbon/silicon composite in the most probable aperture, and its fixed amount is 155mg/ml.
1) 3g F127 is dissolved in 30 of 12ml ethanol and 6.6ml water formation
℃ mixing solutions in.
2) etc. F127 dissolves fully, adds 2.5g Resorcinol, 2.2ml tetraethoxy, is 2M. by adding hydrochloric acid conditioned reaction system HCl concentration
3) continue to add 2.5ml formaldehyde behind the stirring 2h, continuation stirring 4h makes to react completely and carries out under this temperature.
F127 in the reaction system: ethanol: water: Resorcinol: tetraethoxy: the mol ratio of formaldehyde is: 0.024:20:37:2.3:1:2.7.
4) after stirring stops, reaction system is poured into ageing in the culture dish, makes the sample layering.
5) layering sample upper solution is outwelled, again with lower floor's thickness system thermopolymerization 36h. in 120 ℃ baking oven
6) gained sample high-temperature roasting 3h. under 800 ℃ of nitrogen atmospheres being lowered the temperature naturally afterwards, the gained sample is mesoporous carbon/silicon composite.
Gained mesoporous carbon/silicon materials have worm meso-porous duct, and its nitrogen adsorption desorption isotherm is the IV thermoisopleth, illustrate that it is meso-hole structure, and the most probable aperture is that 7.5nm. BET specific surface area is 539.7m
2/ g, pore volume are 0.53cm
3/ g. draws from the EDS energy spectrum analysis, and carbon content is 58.07% in the gained mesoporous material, and to be 13.82%. be applied to the immobilization of N,O-Diacetylmuramidase with gained mesoporous carbon/silicon composite to silicone content, and its fixed amount is 163mg/ml.
1) the reaction system solution temperature remains on 40 ℃, and other are with embodiment 4.
2) concentration adjustment of HCl is 1M in the reaction system, and other are with embodiment 4
3) with embodiment 4
4) with embodiment 4
5) layering sample upper solution is outwelled, again with lower floor's thickness system thermopolymerization 36h. in 120 ℃ baking oven
6) gained sample high-temperature roasting 5h. under 700 ℃ of nitrogen atmospheres being lowered the temperature naturally afterwards, the gained sample is mesoporous carbon/silicon composite.
Gained mesoporous carbon/silicon materials have worm meso-porous duct, measure through the nitrogen adsorption desorption, and gained material B ET specific surface area is 578.7m
2/ g, pore volume are 0.51cm
3/ g, the most probable aperture is 7.6nm.
1) the reaction system solution temperature remains on 40 ℃, and other are with embodiment 4.
2) concentration adjustment of HCl is 1M in the reaction system, and other are with embodiment 4
3) with embodiment 4
4) with embodiment 4
5) layering sample upper solution is outwelled, again with lower floor's thickness system 160
oThermopolymerization 36h. in the baking oven of C
6) gained sample high-temperature roasting 3h. under 800 ℃ of nitrogen atmospheres being lowered the temperature naturally afterwards, the gained sample is mesoporous carbon/silicon composite.
Gained mesoporous carbon/silicon materials have worm meso-porous duct, measure through the nitrogen adsorption desorption, and gained material B ET specific surface area is 552.7m
2/ g, pore volume are 0.54cm
3/ g, the most probable aperture is 7.6nm.
1) 3.78g F127 is dissolved in 50 ℃ the mixing solutions of 11.5ml ethanol and 9ml water formation.
2) etc. F127 dissolves fully, adds 4.4g Resorcinol, 4.4ml tetraethoxy in step 1) solution, and HCl concentration is 0.5M. in the hydrochloric acid conditioning solution by adding
3) continue to stir 2h after, in step 2) add 5ml formaldehyde solution in the solution, under this temperature, continue to stir 4h and make to react completely and carry out.
The F127 that adds in the reaction system: ethanol: water: Resorcinol: tetraethoxy: the mol ratio of formaldehyde is: 0.03:20:50:4:2:5.
4) stir stop after, solution in the step 3) is poured into ageing makes the sample layering in the culture dish.
5) layering sample upper solution in the step 4) is outwelled, again with lower floor's thickness system thermopolymerization 12h. in 160 ℃ baking oven
6) the roasting 5h. under 950 ℃ of nitrogen atmospheres of gained sample in the step 5) being lowered the temperature naturally afterwards, the gained sample is mesoporous carbon/silicon composite.
Gained mesoporous carbon/silicon materials have worm meso-porous duct, and its nitrogen adsorption desorption isotherm is the IV thermoisopleth, illustrate that it is meso-hole structure, and the most probable aperture is that 7.5nm. BET specific surface area is 548.9m
2/ g, pore volume are 0.49cm
3/ g.
1) the reaction system solution temperature remains on 50 ℃, and other are with embodiment 4.
2) concentration adjustment of HCl is 2M in the reaction system, and other are with embodiment 4
3) with embodiment 4
4) with embodiment 4
5) layering sample upper solution is outwelled, again with lower floor's thickness system thermopolymerization 36h. in 160 ℃ baking oven
6) gained sample high-temperature roasting 1h. under 950 ℃ of nitrogen atmospheres being lowered the temperature naturally afterwards, the gained sample is mesoporous carbon/silicon composite.
Gained mesoporous carbon/silicon materials have worm meso-porous duct, measure through the nitrogen adsorption desorption, and gained material B ET specific surface area is 601.8m
2/ g, pore volume are 0.58cm
3/ g, to be 7.7nm. be applied to the immobilization of N,O-Diacetylmuramidase with gained mesoporous carbon/silicon composite in the most probable aperture, and its fixed amount is 201mg/ml.
Claims (1)
1. the preparation method of a mesoporous carbon/silicon composite is characterized in that, may further comprise the steps:
1) F127 is dissolved in 20 ℃ ~ 50 ℃ the mixing solutions of second alcohol and water formation;
2) etc. F127 dissolves fully, adds Resorcinol and tetraethoxy in the mixing solutions of step 1), makes that by adding hydrochloric acid HCl concentration continues to stir 2h between 0.5M ~ 2M in the solution;
3) in step 2) add formaldehyde in the solution that obtains, continue to stir 4h and make to react completely and carry out;
F127 in the reaction system: ethanol: water: Resorcinol: tetraethoxy: the mol ratio of formaldehyde is: 0.01 ~ 0.03:20:20 ~ 50:1 ~ 4:0.5 ~ 2:1 ~ 5;
4) solution that step 3) is obtained is poured into ageing in the culture dish, makes the sample layering;
5) layering sample upper solution in the step 4) is outwelled, again with lower floor's thickness system thermopolymerization 12 ~ 24h in 100 ℃ ~ 160 ℃ baking oven;
6) with gained sample in the step 5) at 600 ℃ ~ 950 ℃ roasting 1 ~ 5h of inert atmosphere, gained sample in cooling back is mesoporous carbon/silicon composite naturally.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104828802A (en) * | 2015-01-19 | 2015-08-12 | 江苏大学 | Synthetic method and application of mesoporous carbon material high-effectively adsorbing tetracycline |
| CN105536879A (en) * | 2015-12-09 | 2016-05-04 | 武汉理工大学 | Low-temperature glue for low-temperature denitration manganese catalyst loading and preparation method of low-temperature glue |
| CN106957056A (en) * | 2017-03-09 | 2017-07-18 | 武汉工程大学 | A kind of synthetic method of the compound feature onion shape mesoporous material of carbon silicon |
| CN108913100A (en) * | 2018-07-30 | 2018-11-30 | 桂林电子科技大学 | A kind of novel ordered mesopore carbon base composite phase-change material and preparation method thereof |
| CN109896516A (en) * | 2019-04-28 | 2019-06-18 | 贵州大学 | A kind of preparation method of the mesoporous Nano carbon balls of situ Nitrogen Doping |
| CN111729512A (en) * | 2020-07-06 | 2020-10-02 | 复旦大学 | Mesoporous carbon-silicon/anodic aluminum oxide composite membrane, super-assembly preparation method and application thereof |
-
2013
- 2013-04-18 CN CN2013101364975A patent/CN103194438A/en active Pending
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| JERZY CHOMA ET AL.: "Soft-templating synthesis and adsorption properties of mesoporous carbons with embedded silver nanoparticles", 《ADSORPTION》 * |
| XIQING WANG ET AL.,: "Facile Synthesis of Ordered Mesoporous Carbons with High Thermal Stability by Self-Assembly of Resorcinol-Formaldehyde and Block Copolymers under Highly Acidic Conditions", 《LANGMUIR》 * |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104828802A (en) * | 2015-01-19 | 2015-08-12 | 江苏大学 | Synthetic method and application of mesoporous carbon material high-effectively adsorbing tetracycline |
| CN105536879A (en) * | 2015-12-09 | 2016-05-04 | 武汉理工大学 | Low-temperature glue for low-temperature denitration manganese catalyst loading and preparation method of low-temperature glue |
| CN105536879B (en) * | 2015-12-09 | 2018-03-16 | 武汉理工大学 | A kind of low-temperature denitration manganese series catalyzer load low temperature glue and preparation method thereof |
| CN106957056A (en) * | 2017-03-09 | 2017-07-18 | 武汉工程大学 | A kind of synthetic method of the compound feature onion shape mesoporous material of carbon silicon |
| CN108913100A (en) * | 2018-07-30 | 2018-11-30 | 桂林电子科技大学 | A kind of novel ordered mesopore carbon base composite phase-change material and preparation method thereof |
| CN109896516A (en) * | 2019-04-28 | 2019-06-18 | 贵州大学 | A kind of preparation method of the mesoporous Nano carbon balls of situ Nitrogen Doping |
| CN111729512A (en) * | 2020-07-06 | 2020-10-02 | 复旦大学 | Mesoporous carbon-silicon/anodic aluminum oxide composite membrane, super-assembly preparation method and application thereof |
| CN111729512B (en) * | 2020-07-06 | 2022-07-29 | 复旦大学 | Mesoporous carbon-silicon/anodic aluminum oxide composite membrane, super-assembly preparation method and application thereof |
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Application publication date: 20130710 |