CN103265007A - Preparation method of ordered mesoporous carbon material containing magnetic metal particles - Google Patents
Preparation method of ordered mesoporous carbon material containing magnetic metal particles Download PDFInfo
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- CN103265007A CN103265007A CN201310178719XA CN201310178719A CN103265007A CN 103265007 A CN103265007 A CN 103265007A CN 201310178719X A CN201310178719X A CN 201310178719XA CN 201310178719 A CN201310178719 A CN 201310178719A CN 103265007 A CN103265007 A CN 103265007A
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Abstract
The invention provides a preparation method of an ordered mesoporous carbon material containing magnetic metal particles. Low-cost and available edible oil is utilized as a carbon source for replacing a process with complex synthesis steps and higher cost. The preparation method comprises the following steps of: firstly dissolving a surfactant and a magnetic metal compound into a hydrochloric organic solvent, adding tetraethyl orthosilicate and stirring, then adding edible oil and stirring, then pouring the mixture into a culture dish, evaporating the organic solvent, then transferring the mixture into a drying oven, and carrying out low temperature polymerization; carrying out high temperature carbonization under the nitrogen atmosphere; and finally grinding and sieving the product, etching silicon oxide by adopting a sodium hydroxide solution with the concentration of 1.0-4.0M, stirring for 6-36 hours, centrifuging and washing to be neutral, repeating grinding and etching processes for 2-6 times, and finally placing the mixture into the drying oven to be dried, thus the ordered mesoporous carbon material containing the magnetic metal particles is obtained. The preparation method has the advantages that a precursor raw material is low in cost, a preparation technology is simple and a process is easy to control, the prepared material is good in ordering, dispersity of the magnetic metal particles is high, and an adsorbing effect is good.
Description
Technical field
The present invention relates to a kind of preparation method who contains magneticmetal particle ordered mesoporous carbon material.Be used for water surrounding micropollutant adsorption separation technology field.
Background technology
Because ordered mesoporous carbon material has aperture, high-specific surface area, high total pore capacities and stable characteristics such as physico-chemical property that homogeneous is easily regulated, makes meso-porous carbon material in technical fields such as absorption, catalysis and support of the catalyst, the energy storage of storage hydrogen, battery electrodes wide application prospect be arranged.And containing magneticmetal particle ordered mesoporous carbon material because of its simple and fast and magnetic resolution performance efficiently, the application in fields such as absorption, catalysis and support of the catalyst has more realistic meaning.At present, the synthetic magneticmetal particle ordered mesoporous carbon material that contains of prior art: prepare the resol ethanolic soln earlier, adopt solvent-induced volatilization self-assembling method to make ordered mesoporous carbon material then.The shortcoming of this method is: synthesis technique complexity, synthetic cost height, processing condition require high; The starting material source is limited, the process control difficulty is big etc.At present existingly syntheticly contain magnetic metal ion ordered mesoporous carbon material method and have a lot of defectives, limited and contain magneticmetal particle ordered mesoporous carbon material in the application of every field.Therefore, invent that simple, the synthetic cost of a kind of preparation technology is low, the starting material wide material sources, building-up process is easy to control, have little composite mesoporous high preparation method who contains magneticmetal particle ordered mesoporous carbon material of double-deck aperture structure, magneticmetal particle dispersity, is the common objective of researcher.
Summary of the invention
The invention discloses a kind of preparation method who contains magneticmetal particle ordered mesoporous carbon material, utilize wide material sources and cheap edible oil, magneticmetal compound, positive tetraethyl orthosilicate, with tensio-active agent under the condition of acidity, carry out solvent evaporates and induce the synthetic meso-porous carbon material that contains the magneticmetal particle of self-assembly, utilize sodium hydroxide solution etching oxidation silicon to obtain containing magneticmetal particle ordered mesoporous carbon material then.Can effectively overcome existing preparation method's synthesis technique complexity, synthetic cost height, processing condition requirement height; Drawbacks such as the starting material source is limited, the process control difficulty is big.
Technical solution of the present invention is achieved in that
A kind of preparation method who contains magneticmetal particle ordered mesoporous carbon material, with the presoma of edible oil as carbon, induce self-assembling method to make itself and tensio-active agent form the synthetic mesoscopic structure carbon material of self-assembly system by the volatilization of organic solvent, dissolve in magneticmetal source and silicon source simultaneously, by high temperature cabonization and etching oxidation silicon, preparation contains magneticmetal particle ordered mesoporous carbon material, it is characterized in that carrying out according to following steps:
(1) with tensio-active agent and magneticmetal compound dissolution in the organic solvent that adds hydrochloric acid, the mol ratio of magneticmetal compound and tensio-active agent is 1:0.1～0.3; Temperature is 20～50 ℃, and the time is 15～30 minutes;
(2) add positive tetraethyl orthosilicate in step (1) product, stir, temperature is 20～50 ℃, and the time is 10～30 minutes;
(3) add edible oil in step (2) product, stir, the mass ratio of edible oil and tensio-active agent is 1:0.1～4.0, and temperature is 30～40 ℃, and the time is 60～240 minutes;
(4) step (3) product is poured in the written instructions culture dish, put into stink cupboard and evaporate organic solvent, the time is 5～8 hours;
(5) step (4) product is moved in the baking oven low temperature polymerization under 80～120 ℃ of conditions, the time is 12～48 hours;
(6) step (5) product is carried out high temperature cabonization under nitrogen protection atmosphere, carbonization temperature is 550～900 ℃, and temperature rise rate is 1～2 ℃/minute, and the time is 1～6 hour;
(7) grinding of step (6) product is sieved, be the sodium hydroxide solution etching oxidation silicon of 1.0～4.0M with concentration, churning time is 6～36h, centrifuge washing is to neutral, repeat this process 2～6 times, put into 60～100 ℃ of dryings of baking oven, make and contain magneticmetal particle ordered mesoporous carbon material.
Edible oil described in the step (3) is any one in soybean oil, Semen Maydis oil, peanut oil, Oleum Gossypii semen, sesame oil, sunflower seed oil, rapeseed oil, the oleum lini.
The magneticmetal compound is any one in six water nickelous nitrates, nine water iron nitrates, cobalt nitrate hexahydrate, the Iron trichloride hexahydrate in the step (1).
The add-on of hydrochloric acid is in the described organic solvent: 0.5～3.0ml, concentration of hydrochloric acid are 0.2mol/L.
The present invention has following advantage and positively effect:
1, the cheap and wide material sources of carbon matrix precursor cost of material are easy to get.
2, preparation technology is simple, does not need to prepare the resol ethanolic soln.
3, preparation process is controlled easily, and conditional request is lower.
4, have little composite mesoporous double-deck aperture structure, have very high specific surface area and total pore capacities.
5, Zhi Bei material order height, magneticmetal particle dispersity height.
6, higher greying, advantages of good adsorption effect have appearred at a lower temperature.
Embodiment
The present invention is described in detail below in conjunction with embodiment, but present embodiment is not limited to the present invention, and every employing similarity method of the present invention and similar variation thereof all should be listed protection scope of the present invention in.
The present invention at first with magneticmetal compound and surfactant dissolves in organic solvent, add a certain amount of hydrochloric acid again and regulate pH, add positive tetraethyl orthosilicate again as the silicon source, add edible oil at last as carbon source, stir and make solvent evaporates induce self-assembly; After treating that solvent volatilizees fully, low temperature polymerization, product at high temperature carries out carbonization and removes tensio-active agent and char-forming material, recycling sodium hydroxide solution etching oxidation silicon, centrifuge washing is to neutral, and cryodrying namely obtains containing magneticmetal particle ordered mesoporous carbon material.
The home-use edible oil of the carbon source material that the present invention uses for buying in market and supermarket, as a kind of with in the herbaceous plant oil of soybean oil, Semen Maydis oil, peanut oil, Oleum Gossypii semen, sesame oil, sunflower seed oil, rapeseed oil, the culinary art of flax wet goods family kitchen, its molecular weight is between 200～500, principal element is C, H, O, also contains elements such as micro-Ca, Mg, K, Na, S, P, Cl.Be preferably soybean oil and Semen Maydis oil.
The tensio-active agent that the present invention uses is the synthetic magneticmetal particle ordered mesoporous carbon material that contains of structure directing agent.The tensio-active agent that uses is water miscible polyoxyethylene～polyoxypropylene～polyoxyethylene (triblock polymer of PEO～PPO～PEO), it is a kind of important amphiphile, amphiphilic molecule, molecular weight is between 5000～20000, and preferred surfactants is P123 (EO20～PO70～EO20) and F127 (EO106～PO70～EO106).Tensio-active agent can be bought from Sigma～Aldrich, and the massfraction of tensio-active agent is 5～10% among the present invention.
Magneticmetal source among the present invention is the water-soluble magnetic metallic compound, and as six water nickelous nitrates, nine water iron nitrates, Iron trichloride hexahydrate, cobalt nitrate hexahydrate etc., these compositions can be randomly dispersed in the mesoscopic structure in self assembling process.Be preferably six water nickelous nitrates and nine water iron nitrates.
Among the present invention, mesoporous material low temperature polymerization in baking oven makes the mesoscopic material formation ordered structure of fully growing, and temperature is 80～120 ℃, and the time is 12～48h; Preferred temperature is 100 ℃, and the preferred time is 24h.
Among the present invention, tensio-active agent and char-forming material structure are removed in mesoporous material high-temperature calcination under protection of inert gas atmosphere, and temperature is 550～900 ℃, and temperature rise rate is 1～2 ℃/minute, and the time is 1～10 hour; Rare gas element is preferably nitrogen or argon gas, and carbonization temperature is preferably 650～850 ℃, and the preferred time is 2～5 hours.
Among the present invention, utilize sodium hydroxide solution etching oxidation silicon to form little composite mesoporous structure, the concentration of sodium hydroxide solution is 1.0～4.0M, and churning time is 6～36h, and multiplicity is 2～6 times; Preferred concentration of sodium hydroxide solution is 2.0M, and preferred churning time is 12h, and preferred multiplicity is 3 times.
Embodiment 1:
Polyoxyethylene～polyoxypropylene～polyoxyethylene (F127) of 1.6g and the nine water iron nitrates of 0.35g are joined in the dehydrated alcohol of 8g, be stirred to dissolving fully, the hydrochloric acid soln that adds the 0.2M of 1.0g again, the positive tetraethyl orthosilicate that slowly adds 2.08g then, after stirring, add the 6.4g Semen Maydis oil and the 8g alcohol mixed solution that stir, stirred 2 hours at 40 ℃; Then product is poured in the culture dish, put into stink cupboard room temperature ethanol evaporation 5～8 hours, put into 100 ℃ baking oven low temperature polymerization 24 hours again; Again product is placed tube furnace, 700 ℃ of high-temperature calcinations are 2 hours under nitrogen protection atmosphere, and temperature rise rate is 2 ℃/minute; Stirring at room 12 hours in the sodium hydroxide solution of 2M then, centrifuge washing repeats this process 3 times to neutral, and 80 ℃ of dryings are 12 hours in baking oven, namely obtain containing magneticmetal particle ordered mesoporous carbon material, are designated as OMC～6.4.
Embodiment 2:
The F127 of 1.6g and the nine water iron nitrates of 0.35g are joined in the dehydrated alcohol of 8g, be stirred to dissolving fully, the hydrochloric acid soln that adds the 0.2M of 1.0g again, the positive tetraethyl orthosilicate that slowly adds 2.08g then, after stirring, add the 4.0g Semen Maydis oil and the 8g alcohol mixed solution that stir, stirred 2 hours at 40 ℃; Then product is poured in the culture dish, put into stink cupboard room temperature ethanol evaporation 5～8 hours, put into 100 ℃ baking oven low temperature polymerization 24 hours again; Again product is placed tube furnace, 700 ℃ of high-temperature calcinations are 2 hours under nitrogen protection atmosphere, and temperature rise rate is 2 ℃/minute; Stirring at room 12 hours in the sodium hydroxide solution of 2M then, centrifuge washing repeats this process 3 times to neutral, and 80 ℃ of dryings are 12 hours in baking oven, namely obtain containing magneticmetal particle ordered mesoporous carbon material, are designated as OMC～4.0.
Embodiment 3:
The F127 of 3.6g and the nine water iron nitrates of 0.35g are joined in the dehydrated alcohol of 8g, be stirred to the hydrochloric acid soln of the 0.2M of dissolving back adding 1.0g fully, the positive tetraethyl orthosilicate that slowly adds 2.08g then, after stirring, add the 2.0g Semen Maydis oil and the 8g alcohol mixed solution that stir, stirred 2 hours at 40 ℃; Then product is poured in the culture dish, put into stink cupboard room temperature ethanol evaporation 5～8 hours, put into 100 ℃ baking oven low temperature polymerization 24 hours again; Again product is placed tube furnace, 700 ℃ of high-temperature calcinations are 2 hours under nitrogen protection atmosphere, and temperature rise rate is 2 ℃/minute; Stirring at room 12 hours in the sodium hydroxide solution of 2M then, centrifuge washing repeats this process 3 times to neutral, and 80 ℃ of dryings are 12 hours in baking oven, namely obtain containing magneticmetal particle ordered mesoporous carbon material, are designated as OMC～2.0.
Embodiment 4:
The F127 of 1.6g and the nine water iron nitrates of 0.35g are joined in the dehydrated alcohol of 8g, be stirred to the hydrochloric acid soln of the 0.2M of dissolving back adding 1.0g fully, the positive tetraethyl orthosilicate that slowly adds 2.08g then, after stirring, add the 1.0g Semen Maydis oil and the 8g alcohol mixed solution that stir, stirred 2 hours at 40 ℃; Then product is poured in the culture dish, put into stink cupboard room temperature ethanol evaporation 5～8 hours, put into 100 ℃ baking oven low temperature polymerization 24 hours again; Again product is placed tube furnace, 700 ℃ of high-temperature calcinations are 2 hours under nitrogen protection atmosphere, and temperature rise rate is 2 ℃/minute; Stirring at room 12 hours in the sodium hydroxide solution of 2M then, centrifuge washing repeats this process 3 times to neutral, and 80 ℃ of dryings are 12 hours in baking oven, namely obtain containing magneticmetal particle ordered mesoporous carbon material, are designated as OMC～1.0.
Embodiment 5:
The F127 of 1.6g and the nine water iron nitrates of 0.35g are joined in the dehydrated alcohol of 8g, be stirred to the hydrochloric acid soln of the 0.2M of dissolving back adding 1.0g fully, the positive tetraethyl orthosilicate that slowly adds 2.08g then, after stirring, add the 0.5g Semen Maydis oil and the 8g alcohol mixed solution that stir, stirred 2 hours at 40 ℃; Then product is poured in the culture dish, put into stink cupboard room temperature ethanol evaporation 5～8 hours, put into 100 ℃ baking oven low temperature polymerization 24 hours again; Again product is placed tube furnace, 700 ℃ of high-temperature calcinations are 2 hours under nitrogen protection atmosphere, and temperature rise rate is 2 ℃/minute; Stirring at room 12 hours in the sodium hydroxide solution of 2M then, centrifuge washing repeats this process 3 times to neutral, and 80 ℃ of dryings are 12 hours in baking oven, namely obtain containing magneticmetal particle ordered mesoporous carbon material, are designated as OMC～0.5.
Embodiment 6:
The F127 of 1.6g and the nine water iron nitrates of 0.35g are joined in the dehydrated alcohol of 8g, be stirred to dissolving fully, add the hydrochloric acid soln of the 0.2M of 1.0g then.The positive tetraethyl orthosilicate that slowly adds 2.08g then after stirring, adds the 0.16g Semen Maydis oil and the 8g alcohol mixed solution that stir, stirs 2 hours at 40 ℃; Then product is poured in the culture dish, put into stink cupboard room temperature ethanol evaporation 5～8 hours, put into 100 ℃ baking oven low temperature polymerization 24 hours again; Again product is placed tube furnace, 700 ℃ of high-temperature calcinations are 2 hours under nitrogen protection atmosphere, and temperature rise rate is 2 ℃/minute; Stirring at room 12 hours in the sodium hydroxide solution of 2M then, centrifuge washing repeats this process 3 times to neutral, and 80 ℃ of dryings are 12 hours in baking oven, namely obtain containing magneticmetal particle ordered mesoporous carbon material, are designated as OMC～0.16.
Embodiment 7:
The F127 of 1.6g and the nine water iron nitrates of 0.16g are joined in the dehydrated alcohol of 8g, be stirred to the hydrochloric acid soln of the 0.2M of dissolving back adding 1.0g fully, the positive tetraethyl orthosilicate that slowly adds 2.08g then, after stirring, add the 1.0g Semen Maydis oil and the 8g alcohol mixed solution that stir, stirred 2 hours at 40 ℃; Then product is poured in the culture dish, put into stink cupboard room temperature ethanol evaporation 5～8 hours, put into 100 ℃ baking oven low temperature polymerization 24 hours again; Again product is placed tube furnace, 700 ℃ of high-temperature calcinations are 2 hours under nitrogen protection atmosphere, and temperature rise rate is 2 ℃/minute; Stirring at room 12 hours in the sodium hydroxide solution of 2M then, centrifuge washing repeats this process 3 times to neutral, and 80 ℃ of dryings are 12 hours in baking oven, namely obtain containing magneticmetal particle ordered mesoporous carbon material.
Embodiment 8:
The F127 of 1.6g and the nine water iron nitrates of 0.50g are joined in the dehydrated alcohol of 8g, be stirred to the hydrochloric acid soln of the 0.2M of dissolving back adding 1.0g fully, the positive tetraethyl orthosilicate that slowly adds 2.08g then, after stirring, add the 1.0g Semen Maydis oil and the 8g alcohol mixed solution that stir, stirred 2 hours at 40 ℃; Then product is poured in the culture dish, put into stink cupboard room temperature ethanol evaporation 5～8 hours, put into 100 ℃ baking oven low temperature polymerization 24 hours again; Again product is placed tube furnace, 700 ℃ of high-temperature calcinations are 2 hours under nitrogen protection atmosphere, and temperature rise rate is 2 ℃/minute; Stirring at room 12 hours in the sodium hydroxide solution of 2M then, centrifuge washing repeats this process 3 times to neutral, and 80 ℃ of dryings are 12 hours in baking oven, namely obtain containing magneticmetal particle ordered mesoporous carbon material.
Embodiment 9:
The F127 of 1.6g and the nine water iron nitrates of 0.35g are joined in the dehydrated alcohol of 8g, be stirred to the hydrochloric acid soln of the 0.2M of dissolving back adding 1.0g fully, the positive tetraethyl orthosilicate that slowly adds 2.08g then, after stirring, add the 1.0g Semen Maydis oil and the 8g alcohol mixed solution that stir, stirred 2 hours at 40 ℃; Then product is poured in the culture dish, put into stink cupboard room temperature ethanol evaporation 5～8 hours, put into 80 ℃ baking oven low temperature polymerization 24 hours again; Again product is placed tube furnace, 700 ℃ of high-temperature calcinations are 2 hours under nitrogen protection atmosphere, and temperature rise rate is 2 ℃/minute; Stirring at room 12 hours in the sodium hydroxide solution of 2M then, centrifuge washing repeats this process 3 times to neutral, and 80 ℃ of dryings are 12 hours in baking oven, namely obtain containing magneticmetal particle ordered mesoporous carbon material.
Embodiment 10:
The F127 of 1.6g and the nine water iron nitrates of 0.35g are joined in the dehydrated alcohol of 8g, be stirred to the hydrochloric acid soln of the 0.2M of dissolving back adding 1.0g fully, the positive tetraethyl orthosilicate that slowly adds 2.08g then, after stirring, add the 1.0g Semen Maydis oil and the 8g alcohol mixed solution that stir, stirred 2 hours at 40 ℃; Then product is poured in the culture dish, put into stink cupboard room temperature ethanol evaporation 5～8 hours, put into 120 ℃ baking oven low temperature polymerization 24 hours again; Again product is placed tube furnace, 700 ℃ of high-temperature calcinations are 2 hours under nitrogen protection atmosphere, and temperature rise rate is 2 ℃/minute; Stirring at room 12 hours in the sodium hydroxide solution of 2M then, centrifuge washing repeats this process 3 times to neutral, and 80 ℃ of dryings are 12 hours in baking oven, namely obtain containing magneticmetal particle ordered mesoporous carbon material.
Embodiment 11:
The F127 of 1.6g and the nine water iron nitrates of 0.35g are joined in the dehydrated alcohol of 8g, be stirred to the hydrochloric acid soln of the 0.2M of dissolving back adding 1.0g fully, the positive tetraethyl orthosilicate that slowly adds 2.08g then, after stirring, add the 1.0g Semen Maydis oil and the 8g alcohol mixed solution that stir, stirred 2 hours at 40 ℃; Then product is poured in the culture dish, put into stink cupboard room temperature ethanol evaporation 5～8 hours, put into 100 ℃ baking oven low temperature polymerization 24 hours again; Again product is placed tube furnace, 550 ℃ of high-temperature calcinations are 2 hours under nitrogen protection atmosphere, and temperature rise rate is 2 ℃/minute; Stirring at room 12 hours in the sodium hydroxide solution of 2M then, centrifuge washing repeats this process 3 times to neutral, and 80 ℃ of dryings are 12 hours in baking oven, namely obtain containing magneticmetal particle ordered mesoporous carbon material.
Embodiment 12:
The F127 of 1.6g and the nine water iron nitrates of 0.35g are joined in the dehydrated alcohol of 8g, be stirred to the hydrochloric acid soln of the 0.2M of dissolving back adding 1.0g fully, the positive tetraethyl orthosilicate that slowly adds 2.08g then, after stirring, add the 1.0g Semen Maydis oil and the 8g alcohol mixed solution that stir, stirred 2 hours at 40 ℃; Then product is poured in the culture dish, put into stink cupboard room temperature ethanol evaporation 5～8 hours, put into 100 ℃ baking oven low temperature polymerization 24 hours again; Again product is placed tube furnace, 900 ℃ of high-temperature calcinations are 2 hours under nitrogen protection atmosphere, and temperature rise rate is 2 ℃/minute; Stirring at room 12 hours in the sodium hydroxide solution of 2M then, centrifuge washing repeats this process 3 times to neutral, and 80 ℃ of dryings are 12 hours in baking oven, namely obtain containing magneticmetal particle ordered mesoporous carbon material.
Embodiment 13:
The F127 of 1.6g and the nine water iron nitrates of 0.35g are joined in the dehydrated alcohol of 8g, be stirred to the hydrochloric acid soln of the 0.2M of dissolving back adding 1.0g fully, the positive tetraethyl orthosilicate that slowly adds 2.08g then, after stirring, add the 1.0g Semen Maydis oil and the 8g alcohol mixed solution that stir, stirred 2 hours at 40 ℃; Then product is poured in the culture dish, put into stink cupboard room temperature ethanol evaporation 5～8 hours, put into 100 ℃ baking oven low temperature polymerization 24 hours again; Again product is placed tube furnace, 700 ℃ of high-temperature calcinations are 1 hour under nitrogen protection atmosphere, and temperature rise rate is 2 ℃/minute; Stirring at room 12 hours in the sodium hydroxide solution of 2M then, centrifuge washing repeats this process 3 times to neutral, and 80 ℃ of dryings are 12 hours in baking oven, namely obtain containing magneticmetal particle ordered mesoporous carbon material.
Embodiment 14:
The F127 of 1.6g and the nine water iron nitrates of 0.35g are joined in the dehydrated alcohol of 8g, be stirred to the hydrochloric acid soln of the 0.2M of dissolving back adding 1.0g fully, the positive tetraethyl orthosilicate that slowly adds 2.08g then, after stirring, add the 1.0g Semen Maydis oil and the 8g alcohol mixed solution that stir, stirred 2 hours at 40 ℃; Then product is poured in the culture dish, put into stink cupboard room temperature ethanol evaporation 5～8 hours, put into 100 ℃ baking oven low temperature polymerization 24 hours again; Again product is placed tube furnace, 700 ℃ of high-temperature calcinations are 6 hours under nitrogen protection atmosphere, and temperature rise rate is 2 ℃/minute; Stirring at room 12 hours in the sodium hydroxide solution of 2M then, centrifuge washing repeats this process 3 times to neutral, and 80 ℃ of dryings are 12 hours in baking oven, namely obtain containing magneticmetal particle ordered mesoporous carbon material.
In the resulting material of above embodiment, be the material that adds 0.015g in the methylene blue solution of 30mg/L to 50ml concentration, in that absorption is after 24 hours under 25 ℃ of conditions, the adsorptive capacity of OMC～0.5 reaches the highest, is 98.01mg/g.OMC～1.0, the adsorptive capacity of OMC～2.0 and OMC～4.0 is respectively 83.73mg/g, 71.74mg/g and 62.44mg/g.Show that the prepared magneticmetal particle ordered mesoporous carbon material that contains of present method has very high saturated extent of adsorption, has good application prospects in the environmental pollutant fractionation by adsorption.
Claims (4)
1. preparation method who contains magneticmetal particle ordered mesoporous carbon material, with the presoma of edible oil as carbon, induce self-assembling method to make itself and tensio-active agent form the synthetic mesoscopic structure carbon material of self-assembly system by the volatilization of organic solvent, dissolve in magneticmetal source and silicon source simultaneously, by high temperature cabonization and etching oxidation silicon, preparation contains magneticmetal particle ordered mesoporous carbon material, it is characterized in that carrying out according to following steps:
(1) with tensio-active agent and magneticmetal compound dissolution in the organic solvent that adds hydrochloric acid, the mol ratio of magneticmetal compound and tensio-active agent is 1:0.1～0.3; Temperature is 20～50 ℃, and the time is 15～30 minutes;
(2) add positive tetraethyl orthosilicate in step (1) product, stir, temperature is 20～50 ℃, and the time is 10～30 minutes;
(3) add edible oil in step (2) product, stir, the mass ratio of edible oil and tensio-active agent is 1:0.1～4.0, and temperature is 30～40 ℃, and the time is 60～240 minutes;
(4) step (3) product is poured in the petri diss, put into stink cupboard and evaporate organic solvent, the time is 5～8 hours;
(5) step (4) product is moved in the baking oven low temperature polymerization under 80～120 ℃ of conditions, the time is 12～48 hours;
(6) step (5) product is carried out high temperature cabonization under nitrogen protection atmosphere, carbonization temperature is 550～900 ℃, and temperature rise rate is 1～3 ℃/minute, and the time is 1～6 hour;
(7) grinding of step (6) product is sieved, be the sodium hydroxide solution etching oxidation silicon of 1.0～4.0M with concentration, churning time is 6～36h, centrifuge washing is to neutral, repeat this process 2～6 times, put into 60～100 ℃ of dryings of baking oven, make and contain magneticmetal particle ordered mesoporous carbon material.
2. a kind of synthetic method that contains magneticmetal particle ordered mesoporous carbon material according to claim 1, it is characterized in that: the edible oil described in the step (3) is any one in soybean oil, Semen Maydis oil, peanut oil, Oleum Gossypii semen, sesame oil, sunflower seed oil, rapeseed oil, the oleum lini.
3. a kind of synthetic method that contains magneticmetal particle ordered mesoporous carbon material according to claim 1 is characterized in that: the magneticmetal compound is any one in six water nickelous nitrates, nine water iron nitrates, cobalt nitrate hexahydrate, the Iron trichloride hexahydrate in the step (1).
4. a kind of synthetic method that contains magneticmetal particle ordered mesoporous carbon material according to claim 1, it is characterized in that: the add-on of hydrochloric acid is in the described organic solvent: 0.5～3.0ml, concentration of hydrochloric acid are 0.2mol/L.
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| CN104163453B (en) * | 2014-07-21 | 2015-08-26 | 复旦大学 | A kind of preparation method of high-sequential nano particle super crystal lattice material |
| CN104167297A (en) * | 2014-08-26 | 2014-11-26 | 桂林电子科技大学 | Tubular mesoporous cobaltosic oxide for super-capacitor and preparation method of tubular mesoporous cobaltosic oxide |
| CN104167297B (en) * | 2014-08-26 | 2018-01-30 | 桂林电子科技大学 | A kind of mesoporous cobaltosic oxide of ultracapacitor tubulose and preparation method thereof |
| CN104528704A (en) * | 2014-12-29 | 2015-04-22 | 上海理工大学 | Preparing method for graphitized ordered mesoporous carbon material |
| CN106450313A (en) * | 2016-11-15 | 2017-02-22 | 安徽安达新能源材料有限公司 | Porous hard-carbon lithium ion battery anode material, preparation method thereof and lithium ion battery |
| CN106450313B (en) * | 2016-11-15 | 2019-10-08 | 宁夏博尔特科技有限公司 | Porous hard carbon lithium ion cell negative electrode material and preparation method thereof and lithium ion battery |
| CN109437152A (en) * | 2018-12-12 | 2019-03-08 | 西北大学 | A kind of preparation method of the nitrogen co-doped meso-porous carbon material of cobalt |
| WO2021121088A1 (en) * | 2019-12-20 | 2021-06-24 | 常州工学院 | Mesoporous carbon material loaded cobalt-based catalyst and preparation method therefor |
| CN111701564A (en) * | 2020-05-26 | 2020-09-25 | 南京财经大学 | Preparation method and application of waste grease magnetic carbon spheres |
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