CN103787305B - Combustion method prepares the method for hollow nano cages - Google Patents
Combustion method prepares the method for hollow nano cages Download PDFInfo
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- CN103787305B CN103787305B CN201410056738.XA CN201410056738A CN103787305B CN 103787305 B CN103787305 B CN 103787305B CN 201410056738 A CN201410056738 A CN 201410056738A CN 103787305 B CN103787305 B CN 103787305B
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- magnesium
- hollow nano
- nano cages
- magnesium oxide
- acid
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The present invention relates to the method that combustion method prepares hollow nano cages, comprising: the magnesium of burning is placed in carbon dioxide atmosphere, make itself and carbon dioxide reaction, collect the ash content burning and obtain, acid adding stirring reaction, to remove magnesium oxide, through washing, drying, obtains hollow nano cages.The magnesium oxide that the present invention utilizes magnesium to burn in carbonic acid gas and obtains is template, to be carbon source prepared solid carbon nano particle being attached in carbonic acid gas on the using magnesium oxide template that burns and obtain with Formed original position during reactive magnesium to carbonic acid gas, then can obtain hollow nano cages with acid removing using magnesium oxide template.Use in this process whole be environmental friendliness reagent, the magnesium salt solution of generation can reclaim, and whole process required equipment is simple, low in raw material price, process are environment friendly and pollution-free, can prepare in a large number.
Description
Technical field
The present invention relates to carbon material, be specifically related to a kind of hollow Nano carbon material and preparation method thereof and the application in fields such as hydrogen reduction.
Background technology
Mesoporous material has large specific surface, large pore volume and homogeneous pore passage structure, is studied widely in many fields such as catalysis, fractionation by adsorption and electrode materialss.Hollow nano cages has large cavity and meso-hole structure due to it, thus is provided with a lot of unique physicochemical property, causes the extensive concern of scientific research personnel.Now, prepare hollow nano cages main method comprise arc process, laser evaporization method, Plasma Polymerization, chemical Vapor deposition process (CVD), supercritical fluid method etc.These methods all need expensive equipment and require complicated and control accurately, and usually need the poisonous or disagreeableness reagent of environment, therefore urgently develop new preparation method.Such as: patent ZL200610024088.6 " method of solid-state preparing great amount of hollow nanometer carbon cage " discloses a kind of method preparing hollow nano cages, for technical field of nanometer material preparation.The amorphous carbon precursor body with the distribution of iron catalyst uniform particle is prepared in this invention first in a large number, then obtains nano cages to heat-treating of presoma by solid state reaction, then hollow nano cages is carried out subsequent disposal and removes catalyzer, namely obtain product.Patent ZL200810023448.X " prepares the method for high-quality nano cages " in a large number and patent 201210062927.9 " a kind of preparation method of N doping hollow nano cages " discloses a kind of bitter earth nano particle produced with magnesium basic carbonate or magnesiumcarbonate decomposition in situ for template, prepares the pure hollow nano cages of high-quality or nitrogen-doped carbon nanocages with benzene, ethanol or pyridine, acetonitrile etc. for carbon source or carbon/nitrogenous source.
Summary of the invention
The object of the invention is to overcome above-mentioned deficiency, provide a kind of combustion method to prepare the method for hollow nano cages.
At this, the invention provides a kind of method that combustion method prepares hollow nano cages, comprising: the magnesium of burning is placed in carbon dioxide atmosphere, make itself and carbon dioxide reaction, collect the ash content burning and obtain, acid adding stirring reaction is to remove magnesium oxide, through washing, drying, obtain hollow nano cages.
The magnesium oxide that the present invention utilizes magnesium to burn in carbonic acid gas and obtains is template, to be carbon source prepared solid carbon nano particle being attached in carbonic acid gas on the using magnesium oxide template that burns and obtain with Formed original position during reactive magnesium to carbonic acid gas, then can obtain hollow nano cages with acid removing using magnesium oxide template.Use in this process whole be environmental friendliness reagent, the magnesium salt solution of generation can reclaim, and whole process required equipment is simple, low in raw material price, process are environment friendly and pollution-free, can prepare in a large number.A kind of new nano cages preparation method.
In the present invention, in preparation process can by select magnesium light the doping that atmosphere realizes hollow nano cages.In one preferred embodiment, lighting atmosphere is air.Like this, the hollow nano cages of gained is doped with N element.
Preferably, ash content burning being obtained falls into the aqueous solution containing doping agent to collect described ash content.In the present invention, by selecting the aqueous solution containing different doping reagent, the doping of different element can be carried out in preparation process.In one preferred embodiment, described doping reagent is the compound containing at least one element in N, B and S.Like this, the hollow nano cages of gained can doped with at least one element in N, B and S.The aqueous solution being dissolved with suitable dopants can be selected as required to collect burning gained ash content, and collection method is simple on the one hand, but also can mix required doped element, the application of expansion gained nano cages.
In a preferred embodiment, described doping reagent is at least one in bicarbonate of ammonia, boric acid and sodium sulphite.
Preferably, in step (3), described acid is hydrochloric acid or dilute sulphuric acid.Preferably, acid adding stirring reaction 12 ~ 36 hours.
The shell of the hollow nano cages of the doping such as nitrogen prepared by the present invention, sulphur, boron has meso-hole structure, there is large specific surface area, there are good hydrogen reduction catalytic performance and stability in the basic conditions, in the field such as ultracapacitor, fuel cell, there is important application prospect.
Accompanying drawing explanation
Fig. 1 is the SEM photo of the hollow nano cages that example according to the present invention prepares, wherein a ~ d corresponding embodiment 1 ~ 4 respectively;
Fig. 2 is the TEM photo of the hollow nano cages that example according to the present invention prepares, wherein a ~ d corresponding embodiment 1 ~ 4 respectively;
The CV curve that Fig. 3 is the hollow nano cages for preparing of example according to the present invention in the saturated potassium hydroxide solution of oxygen/nitrogen, wherein a ~ d corresponding embodiment 1 ~ 4 respectively.
Embodiment
Further illustrate the present invention below in conjunction with accompanying drawing and following embodiment, should be understood that accompanying drawing and following embodiment are only for illustration of the present invention, and unrestricted the present invention.
The present invention is directed in prior art and need expensive equipment and require complicated and control accurately, and the poisonous or disagreeableness problem of environment such as the carbon source used and/or nitrogenous source, provide a kind of method that combustion method prepares hollow nano cages.The magnesium oxide that the present invention utilizes magnesium to burn in carbonic acid gas and obtains is template, and carbonic acid gas is that carbon source has prepared solid carbon nanocages, then can obtain hollow nano cages with acid removing using magnesium oxide template.
Particularly, exemplarily, method of the present invention can comprise the following steps:
Step 1, lights magnesium at least containing the atmosphere of oxygen;
Step 2, is placed in carbon dioxide atmosphere by the magnesium of burning, makes itself and carbon dioxide reaction, and the ash content obtained that burns falls into carbon dioxide atmosphere, water or the aqueous solution;
Step 3, by the solid that obtains and sour stirring reaction, then with deionized water wash repeatedly, centrifugal, dry.
Wherein, in step 1 magnesium light the mixed atmosphere that atmosphere can be air, oxygen or oxygen and other gases.Different lighting atmosphere by selecting, different products of combustion can be produced, thus the hollow nano cages obtained can be made doped with other element.
Preferably, the atmosphere in step 1 is air.Containing magnesium nitride in the products of combustion of such Mg, thus obtained hollow nano cages is doped with N element.
Wherein, the solid obtained that burns in step 2 can fall into air, water or the aqueous solution.Wherein the aqueous solution can be preferably the aqueous solution containing doping reagent, thus the hollow nano cages obtained can be made doped with the element mated with the aqueous solution.The element adulterated includes but not limited at least one in N, B and S.Selected doping reagent includes but not limited to bicarbonate of ammonia, boric acid and/or sodium sulphite.Such as when the aqueous solution is boric acid aqueous solution, sodium sulfide solution respectively can in nano cages doped with boron element, element sulphur.In addition, the concentration of reagent of adulterating in the aqueous solution can be determined according to needing in hollow nano cages the amount of element of adulterating.Preferably, in the aqueous solution, the volumetric molar concentration of doping agent can be 0.05 ~ 0.5mol/L.
Wherein, the acid used in step 3 can be hydrochloric acid, sulfuric acid or other acid can reacted with magnesium oxide.Magnesium oxide in the ash content that its consumption preferably can make burning obtain reacts completely.Like this, can using magnesium oxide template be removed, thus obtain hollow nano cages.The concentration of acid used can be 0.2 ~ 2mol/L, preferably 0.5 ~ 1mol/L.Stirring reaction preferably continues 12 ~ 36 hours, more preferably continues 18 ~ 24 hours.
In addition, the magnesium salt solution that magnesium oxide and acid-respons obtain can reclaim.So both can be environment friendly and pollution-free, can production cost be saved again.
Of the present invention to prepare use in the process of hollow nano cages whole be environmental friendliness reagent, and the magnesium salt solution of generation can reclaim, and whole process required equipment is simple, low in raw material price, process are environment friendly and pollution-free, can prepare in a large number.A kind of new nano cages preparation method.
The hollow nano cages that the present invention prepares except containing except carbon, other elements that can also contain magnesium, nitrogen and/or match with the aqueous solution, such as boron and/or sulphur etc.
Again, the shell of the hollow nano cages that the present invention prepares has meso-hole structure, has the advantages such as specific surface area is large.Its pore volume can be 0.5 ~ 1.5cm
3g
-1, specific surface area can be 200 ~ 500m
2g
-1.Fig. 1 and Fig. 2 illustrates SEM photo and the TEM photo of the hollow nano cages that example according to the present invention prepares respectively.As shown in Figure 1, obtain sample all there is good cubes pattern, carbon cubes a small amount of damaged in SEM photo can find that gained sample has hollow structure; As shown in Figure 2, gained carbon cubes is hollow structure.Fig. 3 illustrates hollow nano cages that example according to the present invention the prepares CV curve in the saturated potassium hydroxide solution of oxygen/nitrogen, and as seen from the figure, the hollow nano cages that the present invention prepares has good hydrogen reduction performance.And it has good hydrogen reduction catalytic performance and stability under acid or alkaline conditions.In addition, this hollow nano cages also has excellent properties such as having extended cycle life, methanol tolerance performance is good.Therefore the fields such as fuel cell can be applied to as oxygen reduction catalyst.
Exemplify embodiment below further to describe the present invention in detail.Should understand equally; following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.The processing parameter etc. that following example is concrete is also only an example in OK range, and namely those skilled in the art can be done in suitable scope by explanation herein and select, and do not really want the concrete numerical value being defined in Examples below.
Embodiment 1
A small amount of water can be added in encloses container one, be full of enough carbonic acid gas.In atmosphere 5 grams of magnesium rods are lighted and it is inserted rapidly in said vesse.After magnesium rod perfect combustion, the ash content that collected by centrifugation falls into the water.The ash obtained is placed in beaker, adds the hydrochloric acid of 10ml0.5mol/L and magnetic agitation.After reaction 24h, by black solid centrifugation wherein, and washing is dry, and can obtain the hollow nano cages of doping nitrogen element, wherein the doping of nitrogen element is 0.5at.%.The aqueous solution of the magnesium salts containing unnecessary hydrochloric acid can reclaim to stay and use it for anything else.The sample prepared has good hydrogen reduction performance, and its CV curve in the saturated potassium hydroxide solution of oxygen/nitrogen is as shown in the figure a in Fig. 3.Its SEM photo and TEM photo are respectively as shown in the figure a in Fig. 1,2, and known its has large cavity and meso-hole structure.Its specific surface area can reach 458m
2g
-1, pore volume can reach 0.98cm
3g
-1.
Embodiment 2
Can add 10mL boric acid aqueous solution in encloses container one, the concentration of its mesoboric acid is 0.1mol/L, is full of enough carbonic acid gas.In atmosphere 5 grams of magnesium rods are lighted and it is inserted rapidly in said vesse.After magnesium rod perfect combustion, collected by centrifugation falls into the ash content of the aqueous solution.The ash obtained is placed in beaker, adds the hydrochloric acid of 10ml0.5mol/L and magnetic agitation.After reaction 24h, by black solid centrifugation wherein, and washing is dry, and can obtain the hollow nano cages of doping nitrogen and boron, wherein the doping of nitrogen element is 0.3at.%, and the doping of boron is 0.8at.%.The aqueous solution of the magnesium salts containing unnecessary hydrochloric acid can reclaim to stay and use it for anything else.The sample prepared has good hydrogen reduction performance, and its CV curve in the saturated potassium hydroxide solution of oxygen/nitrogen is as shown in the figure b in Fig. 3.Its SEM photo and TEM photo are respectively as shown in the figure b in Fig. 1,2, and known its has large cavity and meso-hole structure.Its specific surface area can reach 360m
2g
-1, pore volume can reach 0.8cm
3g
-1.
Embodiment 3
Enough carbonic acid gas can be full of by encloses container one.In atmosphere 5 grams of magnesium rods are lighted and it is inserted rapidly in said vesse.After magnesium rod perfect combustion, collect the ash content falling into container bottom.The ash obtained is placed in beaker, adds the hydrochloric acid of 10ml0.5mol/L and magnetic agitation.After reaction 24h, by black solid centrifugation wherein, and washing is dry, and can obtain the hollow nano cages of doping nitrogen element, wherein the doping of nitrogen element is 0.7at.%.The aqueous solution of the magnesium salts containing unnecessary hydrochloric acid can reclaim to stay and use it for anything else.The sample prepared has good hydrogen reduction performance, and its CV curve in the saturated potassium hydroxide solution of oxygen/nitrogen is as shown in the figure c in Fig. 3.Its SEM photo and TEM photo are respectively as shown in the figure c in Fig. 1,2, and known its has large cavity and meso-hole structure.Its specific surface area can reach 402m
2g
-1, pore volume can reach 0.9cm
3g
-1.
Embodiment 4
Can add 10mL bicarbonate of ammonia and boron aqueous acid in encloses container one, wherein the concentration of bicarbonate of ammonia and boric acid is 0.1mol/L, is full of enough carbonic acid gas.In atmosphere 5 grams of magnesium rods are lighted and it is inserted rapidly in said vesse.After magnesium rod perfect combustion, collected by centrifugation falls into the ash content of the aqueous solution.The ash obtained is placed in beaker, adds the hydrochloric acid of 10ml0.5mol/L and magnetic agitation.After reaction 24h, by black solid centrifugation wherein, and washing is dry, and can obtain the hollow nano cages of doping nitrogen element and boron, wherein the doping of nitrogen element is 0.6at.%, and the doping of boron is 0.5at.%.The aqueous solution of the magnesium salts containing unnecessary hydrochloric acid can reclaim to stay and use it for anything else.The sample prepared has good hydrogen reduction performance, and its CV curve in the saturated potassium hydroxide solution of oxygen/nitrogen is as shown in the figure d in Fig. 3.Its SEM photo and TEM photo are respectively as shown in the figure d in Fig. 1,2, and known its has large cavity and meso-hole structure.Its specific surface area can reach 421m
2g
-1, pore volume can reach 0.93cm
3g
-1.
Industrial applicability: the reagent that method of the present invention uses is environmental friendliness reagent, the magnesium salt solution of generation can reclaim, and whole process required equipment is simple, low in raw material price, process are environment friendly and pollution-free, can prepare in a large number.Obtained nano cages can be applied to the fields such as fuel cell as oxygen reduction catalyst.
Claims (5)
1. a combustion method prepares the method for hollow nano cages, it is characterized in that, comprise: the magnesium of burning is placed in carbon dioxide atmosphere, make itself and carbon dioxide reaction, collect the ash content burning and obtain, acid adding stirring reaction is to remove magnesium oxide, through washing, drying, obtain hollow nano cages, wherein, the ash content that burning is obtained falls into the aqueous solution containing doping agent to collect described ash content.
2. method according to claim 1, is characterized in that, described doping reagent is the compound containing at least one element in N, B and S.
3. method according to claim 2, is characterized in that, described doping reagent is at least one in bicarbonate of ammonia, boric acid and sodium sulphite.
4. according to the method in any one of claims 1 to 3, it is characterized in that, described acid is hydrochloric acid or dilute sulphuric acid.
5. according to the method in any one of claims 1 to 3, it is characterized in that, acid adding stirring reaction 12 ~ 36 hours.
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| CN106006617B (en) * | 2016-05-25 | 2018-04-13 | 广东石油化工学院 | A kind of preparation method and applications of graphene hollow nano cages |
| CN108083255A (en) * | 2017-11-10 | 2018-05-29 | 山东大学 | A kind of preparation method of hollow graphite structure nano cages material |
| CN108417803A (en) * | 2018-03-12 | 2018-08-17 | 华南理工大学 | A kind of N doping hollow carbon sphere composite material and preparation method and application |
| CN109494082A (en) * | 2018-11-19 | 2019-03-19 | 中物院成都科学技术发展中心 | A kind of N doping porous graphite alkenes carbon nanosheet material and its preparation method and application |
| CN113173573B (en) * | 2021-03-04 | 2022-11-08 | 上海大学 | Carbon nanocage material regulated and controlled by carbon quantum dots and preparation method thereof |
| CN113511643B (en) * | 2021-05-14 | 2023-03-21 | 江苏大学 | Method for preparing high-capacitance carbon nanocages in green cycle mode and carbon nanocages |
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