CN101580240A - Method for preparing iron-carrying ordered mesoporous carbon materials - Google Patents
Method for preparing iron-carrying ordered mesoporous carbon materials Download PDFInfo
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- CN101580240A CN101580240A CNA2009100330532A CN200910033053A CN101580240A CN 101580240 A CN101580240 A CN 101580240A CN A2009100330532 A CNA2009100330532 A CN A2009100330532A CN 200910033053 A CN200910033053 A CN 200910033053A CN 101580240 A CN101580240 A CN 101580240A
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Abstract
The invention discloses a method for preparing novel iron-carrying ordered mesoporous carbon materials. Through a soft template route, under the condition of adding no acid additionally, acid produced by iron-salt precursor hydrolysis of a synthesis system is utilized to catalyze phenolic polycondensation, and iron-salt precursors and phenolic polycondensation products are self-assembled around surfactant and are carbonized in inert atmosphere so as to prepare the iron-carrying ordered mesoporous carbon materials. The obtained iron-carrying ordered mesoporous carbon materials are ordered in height, high in specific surface area (410-586m2 . g-1) and uniform in pore size distribution (3.9 nm). The method realizes the one-step synthesis of the iron-carrying ordered mesoporous carbon materials. Compared with mesoporous carbon synthesis through a hard template route and an impregnating-loading process, the method has the advantages of easy operation, low cost, low requirements for equipment, and the like. The iron-carrying ordered mesoporous carbon materials prepared by the method have wide application prospects in the fields of catalysis, separation, electrode materials, repair to environmental pollutants, and the like.
Description
Technical field
The present invention relates to a kind of ordered mesoporous material preparation method's, particularly a kind of iron-carrying ordered mesoporous carbon materials preparation method.
Background technology
Ordered mesoporous carbon material is owing to its regular duct, and bigger specific surface area, the aperture of homogeneous and high stability in many new and high technologies, have important use as fields such as fuel cell, support of the catalyst, transmitter, membrane sepn and are worth.In order further to enlarge the range of application of ordered mesopore carbon, loaded metal in the mesoporous carbon matrix (oxide compound) is nanocrystalline, and the research that forms the mesoporous carbon based composites has caused scientific research personnel's very big attention.The mesoporous carbon based composites is owing to duct and the nanocrystalline distinctive character of loaded metal (oxide compound) that it has the mesoporous carbon rule simultaneously demonstrates a lot of significant performances, after supporting Pt in the orderly mesoporous carbon matrix, it is good electrode materials, can prepare catalyzed reaction electrode efficiently, be applied to energy transformation and transform in the device (fuel cell); Behind orderly supported on carbon surface Ni, demonstrate good magnetic performance in addition, can widen the application of carbon material at magnetic flotation and magnetic catalytic field.At present, to take three kinds of methods in order mesoporous supported on carbon surface master metal.(1) back pickling process: promptly metallics is introduced in the skeleton of the meso-porous carbon material that has prepared by the method for dipping.But the content of metal of this method gained mesoporous carbon based composites is lower, metallic particles is grown greatlyyer, and process is difficult to control; (2) nanometer teeming practice altogether: it is to be hard template with the ordered meso-porous silicon oxide for preparing in advance, the presoma of a certain amount of carbon and metal forerunner salts solution are injected the duct of mesopore silicon oxide, then high temperature cabonization under inert atmosphere is sloughed the silicon oxide template at last.Though this method can be utilized the growth of the confinement effect restriction metal nanoparticle in mesopore silicon oxide duct to a certain extent, step is more loaded down with trivial details; (3) soft template method: this is the nearly 2 years nanocrystalline novel methods of synthesizing ordered mesoporous carbon loaded metal (oxide compound) that occur.This method adopts the self-assembly principle, under acidic conditions, make the self-assembly around nonionogenic tenside of carbon source presoma (phenols and aldehydes) and metal (oxide compound) presoma, obtain the nanocrystalline ordered mesoporous carbon composite material of ordered mesopore carbon loaded metal (oxide compound) through carbonization.This method compares with preceding two kinds of methods that to have process simple, is suitable for the advantage of suitability for industrialized production.At present, people adopt this method to prepare ordered mesopore carbon load TiO
2[R.Liu, Y.Ren, Y.Shi, F.Zhang, L.Zhang, B.Tu, D.Y.Zhao.Chem.Mater.20 (2008) 1140], Ir[P.Gao, A.Wang, X.Wang, T.Zhang.Chem.Mater.20 (2008) 1881.] and Ru[P.Gao, A.W.Wang, X.D.Wang, T.Zhang.Catal.Lett.125 (2008) 289.] matrix material.Although adopt the research of soft template route synthesizing ordered mesoporous carbon loaded metal (oxide compound) to obtain certain progress at present, but existing method all needs to add a certain proportion of mineral acid in preparation process, be used for the polycondensation of catalysis carbon source presoma, preparation process is still comparatively complicated.In addition,, there is important use to be worth in fields such as catalysis, separation and environmental pollution reparations because nanometer metallic iron has good magnetic property and chemically reactive, and the present synthetic report that yet there are no about iron-carrying ordered mesoporous carbon.
Summary of the invention
The purpose of this invention is to provide a kind of under the condition that does not add any acid, the acid that utilizes the hydrolysis of synthetic system molysite presoma to produce comes the polycondensation of catalysis phenolic aldehyde, has the high-sequential structure through soft template route synthetic, bigger than the table surface, homogeneous pore size distribution, and the preparation method of maneuverable iron-carrying ordered mesoporous carbon materials.
The objective of the invention is to be achieved through the following technical solutions, the preparation method of iron-carrying ordered mesoporous carbon materials is characterized in that finishing by following steps:
(1) under the room temperature, the molysite presoma is melted in water/organic solvent mixed solution, obtain solution A, simultaneously, nonionogenic tenside and phenol type substances mixed dissolution in water/organic solvent mixed solution, are obtained solution B;
(2) solution A is slowly joined in the solution B, mixes, react deep purple solution, the reaction times is 1～5 hour;
(3) formaldehyde solution is added in the mixed solution of (2) step, stir and made formaldehyde and the abundant polymerization of phenol type substances in 2-4 hour, stop to stir, mixed solution is divided into two-layer, and the upper strata is a water, and lower floor is an organic phase;
(4) gained two-phase mixed solution is left standstill aging after 60～96 hours, abandoning supernatant, lower floor's organic phase stirs and formed thick liquid in 8-12 hour, through low-temperature curing, gained solid product iron resol-nonionogenic tenside matrix material low-temperature bake under inert atmosphere is removed nonionogenic tenside, handles obtaining iron-carrying ordered mesoporous carbon materials again through high temperature cabonization.
Low-temperature curing temperature described in above-mentioned (4) step is 85 ℃～105 ℃, and the time is 12～48 hours.
Inert atmosphere can be a nitrogen described in above-mentioned (4) step, also can be argon gas.
The temperature that iron content resol described in above-mentioned (4) step-nonionogenic tenside matrix material low-temperature bake is removed tensio-active agent is 350～500 ℃, and temperature rise rate is 1～5 ℃/minute.The carbonization temperature of carrying out high temperature cabonization is 700～900 ℃, roasting 2～3 hours, and temperature rise rate is 1～5 ℃/minute.
Used phenol type substances is a kind of in Resorcinol or the Phloroglucinol among the present invention; Preferred Resorcinol.
Organic solvent among the present invention in institute's water/organic solvent mixed solution is selected from alcohols, and is a kind of for methyl alcohol or alcoholic acid, is preferably ethanol.
The nonionogenic tenside that the present invention uses is polyethylene oxide-poly(propylene oxide)-polyethylene oxide triblock copolymer F127 (EO106PO70EO106).
Used iron content inorganic precursors can be a kind of in iron nitrate and the iron trichloride among the present invention.
It is the iron-carrying ordered mesoporous carbon that soft template synthesizes high-sequential that the present invention adopts tensio-active agent, utilizes the inorganic forerunner's salt hydrolysis of iron content to produce acid and comes the polyreaction of catalysis of phenol class material with formaldehyde, so need not to add acid source in the reaction system.Its dominant mechanism is: in the mixed solution of water/organic solvent, the acid catalysis phenol type substances that the inorganic forerunner's salt hydrolysis of iron content produces is given birth to reaction with oxymethylene polymerization, and generate ferruginous phenol type substances-yuban simultaneously, that utilizes this polymkeric substance and nonionogenic tenside then have-and machine-organic self-assembly obtains iron content resol-nonionogenic tenside matrix material, low-temperature bake is removed tensio-active agent under the inert atmosphere, promptly obtain the iron content ordered mesoporous polymer, further carbonization obtains the iron-carrying ordered mesoporous carbon materials of corresponding construction.
The preparation method of iron-carrying ordered mesoporous carbon materials of the present invention compares its significant effect with the preparation process of traditional metal load ordered mesoporous carbon composite material: 1) need not add under the condition of any acid, the acid that utilizes the hydrolysis of synthetic system molysite presoma to produce comes the polycondensation of catalysis phenolic aldehyde, through the synthetic iron-carrying ordered mesoporous carbon materials of soft template route, simplified the building-up process of iron-carrying ordered mesoporous carbon; Simple to operate, cost is low, and equipment requirements is easy; 2) iron mainly exists with the form of fe in its hole wall of iron-carrying ordered mesoporous carbon materials of making of the present invention, and mainly exists with the form of ferric oxide at the surperficial iron of carbon.This is Zero-valent Iron easy oxidized the causing in air owing to the surface, and surface oxidation iron and mesoporous carbon structure have played the certain protection effect to the fe in the hole wall, and it is oxidized that it is difficult for; 3) the duct high-sequential of iron-carrying ordered mesoporous carbon materials, specific surface area is big, the pore size distribution homogeneous; The specific surface area of this iron-carrying ordered mesoporous carbon materials is 358-586m
2G
-1, pore volume is 0.28-0.41cm
3G
-1, the aperture is 3.9nm.Iron-carrying ordered mesoporous material according to this method makes has broad application prospects in the fields such as reparation of catalysis, separation, electrode materials and environmental pollutant.
Concrete preparation process of the present invention is provided by following examples.
Embodiment
Below selecting the different add-ons of molysite presoma in the reaction, and to adopt the magnetic agitation pattern be example, in conjunction with specific embodiments, the present invention described in further detail.
Protection scope of the present invention is not limited to following examples, and enumerating these examples only is in order to set forth rather than limit by any way the present invention.
Embodiment 1
The first step: under the room temperature, select the Fe (NO of 0.303g
3)
39H
2O is dissolved in water/alcohol mixed solution as the molysite presoma, it is stand-by that magnetic agitation obtains settled solution A, select the nonionogenic tenside F127 of 2.5g and the Resorcinol of 1.65g to be dissolved in the mixing solutions of water/ethanol (volume ratio 1/1) again, magnetic agitation obtains being bright brown solution B; Second step: what will prepare is dissolved with 0.303gFe (NO
3)
39H
2The water of O/alcohol mixed solution A slowly adds among the mixing solutions B of F127 and Resorcinol, mixes 1 hour, obtains solution after the reaction and is intense violet color; The 3rd step: the formaldehyde solution of 2.5g37% is added in the mixed solution in above-mentioned second step, continued to mix 3 hours, after making the abundant polymerization of phenolic aldehyde, stop to stir, mixed solution is divided into two-layer up and down gradually, the upper strata be water with ethanol mutually, lower floor is the compound phase of iron content resol-nonionogenic tenside; The 4th step: above-mentioned two-phase mixed solution room temperature was left standstill 60 hours, abandoning supernatant, again the compound phase mixed solution of lower floor's iron content resol-nonionogenic tenside was stirred 8 hours, be transferred to 85 ℃ of curing ovens at last after 12 hours, product 700 ℃ of roastings under nitrogen atmosphere were promptly obtained the iron-carrying ordered mesoporous carbon materials of hexagonal structure in 2 hours, temperature rise rate be 20-350 ℃ (1 ℃/min), 350-700 ℃ (5 ℃/min).The aperture of this iron-carrying ordered mesoporous carbon materials is 3.9nm, and pore volume is 0.32cm
3G
-1, specific surface area is 452m
2G
-1
Embodiment 2
Reactions steps and embodiment 1 are identical, and difference is to select Fe (NO3) 39H2O of 0.606g as the molysite presoma; To time of mixing of containing the mixing solutions of solution A and solution B in second step be 3 hours, the time of mixing of continuing that adds after the formaldehyde solution is 2 hours; Last two-phase mixed solution room temperature left standstill 72 hours, restir 24 hours, be transferred to 100 ℃ of curing ovens at last after 12 hours, product 800 ℃ of roastings under nitrogen atmosphere were promptly obtained the iron-carrying ordered mesoporous carbon materials of hexagonal structure in 2 hours, temperature rise rate be 20-400 ℃ (1 ℃/min), 400-800 ℃ (5 ℃/min).The aperture of the iron-carrying ordered mesoporous carbon materials that obtains is 3.9nm, and pore volume is 0.41cm3g-1, and specific surface area is 586m2g-1.
Embodiment 3
Reactions steps and embodiment 1 are identical, and difference is to select the FeCl3 of 0.365g as the molysite presoma; Second step: the water that the is dissolved with 0.365g FeCl3/methanol mixed solution A that will prepare slowly adds among the mixing solutions B of F127 and Phloroglucinol, and the time of mixing of containing the mixing solutions of solution A and solution B in going on foot second is 5 hours; The time of mixing of continuing after the adding formaldehyde solution is 2 hours; Last two-phase mixed solution room temperature left standstill 96 hours, restir 10 hours, be transferred to 105 ℃ of curing ovens at last after 24 hours, product 800 ℃ of roastings under argon gas atmosphere were promptly obtained the iron-carrying ordered mesoporous carbon materials of hexagonal structure in 3 hours, temperature rise rate be 20-500 ℃ (1 ℃/min), 500-900 ℃ (5 ℃/min).The aperture of the iron-carrying ordered mesoporous carbon materials that obtains is 3.9nm, and pore volume is 0.28cm3g-1, and specific surface area is 358m2g-1.
In above-mentioned each example reaction, can control the content of iron in the final product by the concentration that changes molysite in the solution A.
Claims (6)
1, a kind of preparation method of iron-carrying ordered mesoporous carbon materials is characterized in that it is to finish according to following steps: under (1) room temperature, the molysite presoma is melted in water/organic solvent mixed solution, obtain solution A; Simultaneously, nonionogenic tenside and phenol type substances mixed dissolution in water/organic solvent mixed solution, are obtained solution B;
(2) solution A is slowly joined in the solution B, mixes, react deep purple solution, the reaction times is 1～5 hour;
(3) formaldehyde solution is added in the mixed solution of (2) step, stirred 2-4 hour, make the abundant polymerization of formaldehyde and phenol type substances, stop to stir, mixed solution is divided into two-layer, and the upper strata is a water, and lower floor is an organic phase;
(4) gained two-phase mixed solution is left standstill aging after 60～96 hours, abandoning supernatant, lower floor's organic phase stirs and formed thick liquid in 8-12 hour, through low-temperature curing, gained solid product iron resol-nonionogenic tenside matrix material low-temperature bake under inert atmosphere is removed nonionogenic tenside, handles obtaining iron-carrying ordered mesoporous carbon materials again through high temperature cabonization.
2, according to the preparation method of the described iron-carrying ordered mesoporous carbon materials of claim 1, it is characterized in that low-temperature curing temperature described in above-mentioned (4) step is 85 ℃～105 ℃, the time is 12～48 hours; Inert atmosphere can be a nitrogen, also can be argon gas; The temperature that iron content resol-nonionogenic tenside matrix material low-temperature bake is removed tensio-active agent is 350～500 ℃, temperature rise rate is 1～5 ℃/minute, the carbonization temperature of carrying out high temperature cabonization is 700～900 ℃, roasting 2～3 hours, and temperature rise rate is 1～5 ℃/minute.
3,, it is characterized in that used phenol type substances is a kind of in Resorcinol or the Phloroglucinol according to the preparation method of the described iron-carrying ordered mesoporous carbon materials of claim 1; Preferred Resorcinol.
4, according to the preparation method of the described iron-carrying ordered mesoporous carbon materials of claim 1, it is characterized in that the organic solvent in used water/organic solvent mixed solution is selected from alcohols, a kind of for methyl alcohol or alcoholic acid, be preferably ethanol.
5,, it is characterized in that the nonionogenic tenside that uses is polyethylene oxide-poly(propylene oxide)-polyethylene oxide triblock copolymer F127 (EO106PO70EO106) according to the preparation method of the described iron-carrying ordered mesoporous carbon materials of claim 1.
6,, it is characterized in that used iron content inorganic precursors can be a kind of in iron nitrate and the iron trichloride according to the preparation method of the described iron-carrying ordered mesoporous carbon materials of claim 1.
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|---|---|---|---|---|
| CN101823777A (en) * | 2010-04-20 | 2010-09-08 | 上海大学 | Method for removing phenol in aqueous solution with magnetic mesoporous carbon material |
| CN101891187A (en) * | 2010-07-26 | 2010-11-24 | 南京理工大学 | Low-temperature soft template one-step synthesis method for graphitized ordered mesoporous carbon material |
| CN103232125A (en) * | 2013-05-13 | 2013-08-07 | 山东大学 | Method for removing bromate through ordered mesoporous carbon loaded nanoscale zero-valent iron material |
| TWI504560B (en) * | 2010-08-06 | 2015-10-21 | Delta Electronics Inc | Manufacturing process for porous material |
| CN105110424A (en) * | 2015-08-18 | 2015-12-02 | 昆明理工大学 | Preparation method for floatable nano mesoporous zero-valent iron carbon material |
| CN105536783A (en) * | 2015-12-23 | 2016-05-04 | 上海大学 | A preparing method of an ordered mesoporous carbon-supported Ru nanometer catalyst |
| CN105842288A (en) * | 2016-03-22 | 2016-08-10 | 苏州捷德瑞精密机械有限公司 | Porous gas sensitive nanomaterial and preparation method thereof |
| CN106241884A (en) * | 2016-07-15 | 2016-12-21 | 上海应用技术学院 | A kind of preparation method and applications of mesoporous iron oxide nano material |
| CN107394174A (en) * | 2017-07-28 | 2017-11-24 | 鲁东大学 | A kind of preparation method of iron oxide mesoporous carbon lithium ion battery negative material |
| CN108314006A (en) * | 2018-04-23 | 2018-07-24 | 北方民族大学 | A kind of ordered mesoporous carbon material and preparation method thereof |
| CN109304143A (en) * | 2018-11-21 | 2019-02-05 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of meso-porous carbon material of load iron and products thereof and application |
| CN110075844A (en) * | 2019-04-30 | 2019-08-02 | 上海师范大学 | Nanometer iron-based fischer-tropsch synthetic catalyst of mesoporous carbon-loaded and its preparation method and application |
| CN111604051A (en) * | 2020-06-19 | 2020-09-01 | 农业农村部环境保护科研监测所 | Lignin-based ordered mesoporous carbon catalyst and preparation method and application thereof |
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| CN115025797A (en) * | 2022-05-23 | 2022-09-09 | 南京工业大学 | Metal carbon nitrogen layer coated ordered mesoporous carbon catalytic material with core-shell structure and preparation method and application thereof |
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| CN100519411C (en) * | 2006-12-29 | 2009-07-29 | 上海师范大学 | Synthesis of high mechanical stability non-metal element doped ordered mosopore carbon material |
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- 2009-06-11 CN CN2009100330532A patent/CN101580240B/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101823777A (en) * | 2010-04-20 | 2010-09-08 | 上海大学 | Method for removing phenol in aqueous solution with magnetic mesoporous carbon material |
| CN101823777B (en) * | 2010-04-20 | 2011-12-21 | 上海大学 | Method for removing phenol in aqueous solution with magnetic mesoporous carbon material |
| CN101891187A (en) * | 2010-07-26 | 2010-11-24 | 南京理工大学 | Low-temperature soft template one-step synthesis method for graphitized ordered mesoporous carbon material |
| TWI504560B (en) * | 2010-08-06 | 2015-10-21 | Delta Electronics Inc | Manufacturing process for porous material |
| CN103232125A (en) * | 2013-05-13 | 2013-08-07 | 山东大学 | Method for removing bromate through ordered mesoporous carbon loaded nanoscale zero-valent iron material |
| CN105110424A (en) * | 2015-08-18 | 2015-12-02 | 昆明理工大学 | Preparation method for floatable nano mesoporous zero-valent iron carbon material |
| CN105536783A (en) * | 2015-12-23 | 2016-05-04 | 上海大学 | A preparing method of an ordered mesoporous carbon-supported Ru nanometer catalyst |
| CN105842288A (en) * | 2016-03-22 | 2016-08-10 | 苏州捷德瑞精密机械有限公司 | Porous gas sensitive nanomaterial and preparation method thereof |
| CN106241884A (en) * | 2016-07-15 | 2016-12-21 | 上海应用技术学院 | A kind of preparation method and applications of mesoporous iron oxide nano material |
| CN107394174A (en) * | 2017-07-28 | 2017-11-24 | 鲁东大学 | A kind of preparation method of iron oxide mesoporous carbon lithium ion battery negative material |
| CN108314006A (en) * | 2018-04-23 | 2018-07-24 | 北方民族大学 | A kind of ordered mesoporous carbon material and preparation method thereof |
| CN109304143A (en) * | 2018-11-21 | 2019-02-05 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of meso-porous carbon material of load iron and products thereof and application |
| CN109304143B (en) * | 2018-11-21 | 2021-09-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of iron-loaded mesoporous carbon material, product and application thereof |
| CN110075844A (en) * | 2019-04-30 | 2019-08-02 | 上海师范大学 | Nanometer iron-based fischer-tropsch synthetic catalyst of mesoporous carbon-loaded and its preparation method and application |
| CN111604051A (en) * | 2020-06-19 | 2020-09-01 | 农业农村部环境保护科研监测所 | Lignin-based ordered mesoporous carbon catalyst and preparation method and application thereof |
| CN111604051B (en) * | 2020-06-19 | 2023-03-10 | 农业农村部环境保护科研监测所 | Lignin-based ordered mesoporous carbon catalyst and preparation method and application thereof |
| CN112028063A (en) * | 2020-07-31 | 2020-12-04 | 珠海复旦创新研究院 | Porous graphene material |
| CN113877580A (en) * | 2021-09-10 | 2022-01-04 | 南开大学 | Fe0Base-ordered mesoporous carbon electrocatalyst and preparation method and application thereof |
| CN115025797A (en) * | 2022-05-23 | 2022-09-09 | 南京工业大学 | Metal carbon nitrogen layer coated ordered mesoporous carbon catalytic material with core-shell structure and preparation method and application thereof |
| CN115501864A (en) * | 2022-10-26 | 2022-12-23 | 广州欣旺科技有限公司 | Biomass porous adsorbent for waste gas treatment and preparation method thereof |
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