CN106276856A - A kind of preparation method of porous carbon Quito component nano composite material - Google Patents
A kind of preparation method of porous carbon Quito component nano composite material Download PDFInfo
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- CN106276856A CN106276856A CN201610657481.2A CN201610657481A CN106276856A CN 106276856 A CN106276856 A CN 106276856A CN 201610657481 A CN201610657481 A CN 201610657481A CN 106276856 A CN106276856 A CN 106276856A
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- porous carbon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The invention discloses the preparation method of a kind of porous carbon Quito component nano composite material, comprise the following steps: the natural biologic material with fine graded porous structure is carried out pretreatment to be used as template；By step impregnation and the atmosphere calcination processing of metal salt solution, the prepared porous carbon with biological template fine hiberarchy is matrix the multicomponent composite materials loading heterogeneity nano unit.The template that the inventive method is used is from the natural biologic material being extensively easy to get and can directly provide carbon source, by selecting different metal salt solutions, regulate and control different dipping process and the technological parameter of calcination process, it is possible to achieve multicomponent mixture and fine micro-nano hierarchy to final composite are controlled.The preparation method of the present invention is simple to operate, with low cost, and the most controlled, and its obtained nano composite material has broad application prospects in fields such as catalysis, sensing, lithium electricity.
Description
Technical field
The present invention relates to the preparation method of a kind of multicomponent nanocomposite composite, particularly relate to a kind of classifying porous to have
The material with carbon element of structure carries out compound institute as matrix, dissimilar metals and metallic compound nano structure on porous carbon matrix
The preparation method of the porous carbon Quito component nano composite material formed, belongs to C-base composte material technical field.
Background technology
The industrial technology of modern civilization is that human lives provides the product of abundance and brings great convenience, and deposits also
In the environmental problem such as such as air pollution, water pollution, efficiency of energy utilization be low.How to prepare can efficient detection gas, rush
Enter environment-friendly materials, raising efficiency of energy utilization that pollutant are effectively degraded, especially realize material when facing multiple environmental problem
The function of material is integrated, is a kind of process of current this research field urgent need.
For in the many multi-functional nanometer materials being applied to environmental problem, usually because component single and apply in reality
During run into a lot of obstacle.With semi-conducting material SnO2As a example by, apply at sensory field, because of SnO2Activity is the highest makes it right
When some gases detect, there is significant limitation in Gas-sensing measurment and selectivity, thus limits the range of its application
And the degree of depth；Apply in photocatalysis field, due to its energy gap 3.6eV, belong to wide band gap semiconducter, only with in sunlight
The ultraviolet portion less than 4%, thus seriously constrain the performance of photocatalysis performance.Therefore, it is necessary to pass through material composition
Compound, preparation various ingredients intercouples the nano material coexisted.
On the other hand, there is high-specific surface area, and be provided that the classification in more avtive spot and active transmission duct is many
Pore structure is conducive to improving the sensing character of material, absorbability and catalysis activity etc., therefore obtains that to have micro-nano classifying porous
Structure is an up the important channel of composite property.For the preparation of classifying porous material, the most conventional method, such as: gas
Phase sedimentation, solution vapour deposition method, method of electrostatic spinning etc. have been carried out some and attempt and explore.But, these preparation methoies at present
Generally require by specific experimental facilities with means, carry out under conditions of relatively harsh, the more difficult control of preparation process, especially
It is difficult to effectively controlling of fine graded porous structure and being combined of various ingredients.
And, porous carbon based composites is owing to having excellent capacitive properties, lithium electrical property, sensing character etc. more
Field has significant application value and day by day causes extensive concern and attention.First, carbon base body can be as the height of transmission electronics
Speed passage, promotes and transmits energy and the performance of information in electronic transmission process.Secondly, carbon relies on its high temperature resistant, low-density and heat
The coefficient of expansion is little waits excellent properties, makes the micro-nano structure of material to keep relative stability, and provides raw for other component materials
Long matrix.Furthermore, component modification is implemented in the introducing of carbon, thus improves the performance of composite.Find through retrieval, close
Many patent disclosure are had, " a kind of manganese oxide/carbon/CNT as entitled in publication number CN105702923A in c-based nanomaterial
Nano-hybrid material and its preparation method and application " patent in, manganese oxide precursor solution is dispersed in thermosetting resin list
In body solvent, this resin monomer can be used simultaneously as carbon source；Then introducing CNT, the solid after being solidified by double bond is through powder
Obtain after broken, high-temperature calcination, but this method is not provided that fine pore space structure；Publication number CN102951677A is entitled
In the patent of " method preparing stannic oxide micro-nano rice material based on aumospheric pressure cvd method ", its prepare carbonaceous material with
The process of nanometer titanium dioxide tin composite is complicated, and lacks obvious advantage in application aspect.
Summary of the invention
Preparing the deficiency of fine micro-nano structure composite for prior art, and porous carbon based composites compel
Cutting application demand, the preparation method of the present invention selects have the biomaterial of particular hierarchical loose structure type as carbon base body
Source, as a example by Pollen Brassicae campestris, based on biological template method, step impregnation technology and atmosphere calcine technology, first to natural biological
Template carries out pre-treatment and activation, then through substep repeatedly impregnation process, then carries out control climate calcination processing, prepares porous carbon back
Multicomponent nanocomposite composite.The preparation method technical process of the present invention is simple, reliability is high, with low cost, difference can be realized
Plant metal and metal compound material being effectively combined on classifying porous carbon base body, it is possible to by adjusting dipping process and forging
The technological parameter of burning process is to control the features such as composition and the micro-nano hierarchy of final composite, it is achieved high-performance porous carbon
The controlled preparation of Quito component nano composite material.The porous carbon base multicomponent nanocomposite prepared according to the preparation method of the present invention is multiple
Condensation material has broad application prospects in fields such as air-sensitive, photocatalysis, battery, super capacitors.
The concrete technical scheme of the present invention is as follows:
The preparation method of a kind of porous carbon Quito component nano composite material, comprises the following steps:
1) select there is the natural biologic material of loose structure as template, and template is carried out pretreatment；
2) template is sequentially placed in the first impregnation liquid and the second impregnation liquid and carries out repeatedly step impregnation, take after having impregnated
Go out template and carry out cleaning and being dried；
3) template is carried out atmosphere calcining, prepare porous carbon Quito component nano composite material.Multicomponent refers to different
Metal simple-substance and metallic compound.
Preferably, template refers to have fine graded porous structure and be provided that abundant carbon source is for preparing porous carbon matrix
Natural biologic material.Such as, pollen.
Preferably, pretreatment refers to: template is placed in ethanol and carries out sonic oscillation or stir process, then cleaning is dried.
Pretreatment is in order to remove the mineral impurity in natural biologic material, and dredges its loose structure, and obtains active bio
Template.The purpose of pretreatment is active natural biomaterial, so the mode of pretreatment is not limited to this, as long as activation can be realized
Method.
Preferably, the first impregnation liquid refer to the inorganic salt solution of precious metal ion, the first impregnation liquid be concentration 0.05～
The ethanol solution of 0.5mmol/L or aqueous solution.It is highly preferred that precious metal ion includes the one in palladium, platinum, gold, silver, copper or several
The combination planted.
Preferably, the second impregnation liquid refer to the inorganic salt solution of transition metal ions, the second impregnation liquid be concentration 0.01～
The ethanol solution of 0.1mol/L or aqueous solution.It is highly preferred that the inorganic salt of transition metal ions include stannum, antimony, zinc, ferrum, cobalt,
The combination of one or more in nickel, indium, the nitrate of cerium, hydrochlorate, sulfate, sulfide.
Preferably, the mixed gas that atmosphere is air, nitrogen or oxygen and nitrogen that atmosphere calcining uses.Mixed gas
Middle oxygen is 20:80～0:100 with the volume range of nitrogen.The calcine technology of atmosphere calcining is: the heating rate of 1～10 DEG C
Rise to 400～700 DEG C calcine.
Accompanying drawing explanation
Fig. 1 is the porous carbon Quito component nano composite material prepared with pollen for template in embodiments of the invention 1
SEM schemes；
Fig. 2 is the porous carbon Quito component nano composite material prepared with pollen for template in embodiments of the invention 1
HRTEM schemes.
Detailed description of the invention
In embodiments of the present invention, after biological template is carried out pre-treatment and activation, use step impregnation, more cleaned, dry
Dry, finally use atmosphere calcining etc. to process step, prepare porous carbon Quito component nano composite material.
Embodiment 1
The purchase Pollen Brassicae campestris from Wang Shi Mel garden is taken 5g be dissolved in about 100ml dehydrated alcohol, Under Ultrasonic Vibration under 40kHz
Swing and clean after 5min, then clean after sonic oscillation 25min under 40kHz, sucking filtration after room temperature 1000r/min magnetic agitation 5min,
Clean, 2 times the most repeatedly, natural drying.Take 0.05mmol PdCl2It is molten that powder is dissolved in 100ml dehydrated alcohol formation supersaturation
Liquid, regulates its pH=6, then sucking filtration, takes upper strata clarification saturated solution, for single-steeping solution.By pollen leaching good for pretreatment
Enter in above single-steeping liquid, with 1000r/min magnetic agitation 15h, then sucking filtration, clean, be dried, lucifuge kept dry is one
Secondary impregnation product.Single-steeping product is immersed the SnCl of 0.04mol/L4·5H2In O ethanol solution, with 1000r/min magnetic force
Stirring 8h, then sucking filtration, clean, be dried, lucifuge kept dry is double-steeping product.By double-steeping product in volume ratio it is
The N of 1:12-O2Under atmosphere, it is raised to 400 DEG C of calcining 2h with 2 DEG C/min heating rate, then cools to room temperature with the furnace, prepare classification
Porous carbon Quito component nano composite material, wherein carbon base body remains the graded porous structure of pollen template, metal simple-substance Pd
Crystallite dimension be 2.5nm, PdO crystallite dimension be 2nm, SnO2Crystallite dimension is 4.5nm, and various nanocrystals are equal on carbon base body
Even distribution.
The present embodiment obtained product having done SEM and EDS test and has analyzed, result see table the figure of 1 and Figure of description
1.Fig. 1 is the SEM figure of the porous carbon Quito component nano composite material prepared with pollen for template in the present embodiment；Table 1 is this
The EDS power spectrum result of the Fig. 1 of the porous carbon Quito component nano composite material prepared with pollen for template in embodiment.
Table 1
Embodiment 2
The purchase Pollen Brassicae campestris from Wang Shi Mel garden is taken 5g be dissolved in about 100ml dehydrated alcohol, Under Ultrasonic Vibration under 40kHz
Clean after swinging 5min, then clean after sonic oscillation 25min under 40kHz, take out after room temperature 1000r/min magnetic agitation 5min afterwards
Filter, cleaning, 2 times the most repeatedly, natural drying.Take 0.05mmol PdCl2Powder is dissolved in 100ml dehydrated alcohol formation satiety
And solution, regulate its pH=8, then sucking filtration, take upper strata clarification saturated solution, for single-steeping solution.The flower good by pretreatment
Powder immerses in above single-steeping liquid, with 1000r/min magnetic agitation 15h, then sucking filtration, clean, be dried, lucifuge kept dry
For single-steeping product.Single-steeping product is immersed the SnCl of 0.04mol/L4·5H2In O ethanol solution, with 1000r/min
Magnetic agitation 8h, then sucking filtration, clean, be dried, lucifuge kept dry is double-steeping product.By double-steeping product at nitrogen
Under protection, it is raised to 500 DEG C of calcining 2h with 2 DEG C/min heating rate, then cools to room temperature with the furnace under nitrogen protection, prepare classification
Porous carbon Quito component nano composite material, wherein carbon base body remains the graded porous structure of pollen template, metal simple-substance Pd
Crystallite dimension be 3nm, PdO crystallite dimension be 2nm, SnO2Crystallite dimension is 5nm, and various nanocrystals uniformly divide on carbon base body
Cloth.
Embodiment 3
The purchase Pollen Brassicae campestris from Wang Shi Mel garden is taken 5g be dissolved in about 100ml dehydrated alcohol, Under Ultrasonic Vibration under 40kHz
Clean after swinging 5min, then clean after sonic oscillation 25min under 40kHz, take out after room temperature 1000r/min magnetic agitation 5min afterwards
Filter, cleaning, 2 times the most repeatedly, natural drying.Take 0.05mmol PdCl2Powder is dissolved in 100ml dehydrated alcohol formation satiety
And solution, regulate its pH=8, then sucking filtration, take upper strata clarification saturated solution, for single-steeping solution.The flower good by pretreatment
Powder immerses in above single-steeping liquid, with 1000r/min magnetic agitation 15h, then sucking filtration, clean, be dried, lucifuge kept dry
For single-steeping product.Single-steeping product is immersed the SnCl of 0.04mol/L4·5H2In O ethanol solution, with 1000r/min
Magnetic agitation 8h, then sucking filtration, clean, be dried, lucifuge kept dry is double-steeping product.By double-steeping product at volume
Than the N for 2:12-O2Under atmosphere, it is raised to 600 DEG C of calcining 2h with 2 DEG C/min heating rate, then cools to room temperature with the furnace, preparation
Graded porous carbon Quito component nano composite material, wherein carbon base body remains the graded porous structure of pollen template, metal list
Matter Pd crystallite dimension be 3nm, PdO crystallite dimension be 2.5nm, SnO2Crystallite dimension is 5.5nm, and various nanocrystals are at carbon base body
On be uniformly distributed.
The preferred embodiment of the present invention described in detail above.Should be appreciated that those of ordinary skill in the art without
Need creative work just can make many modifications and variations according to the design of the present invention.Therefore, all technology in the art
Personnel are available by logical analysis, reasoning, or a limited experiment the most on the basis of existing technology
Technical scheme, all should be in the protection domain being defined in the patent claims.
Claims (10)
1. the preparation method of porous carbon Quito component nano composite material, it is characterised in that comprise the following steps:
1) select there is the natural biologic material of loose structure as template, and described template is carried out pretreatment；
2) described template is sequentially placed in the first impregnation liquid and the second impregnation liquid carries out repeatedly step impregnation, take after having impregnated
Go out described template and be carried out and be dried；
3) described template is carried out atmosphere calcining, prepare described porous carbon Quito component nano composite material.
The preparation method of a kind of porous carbon Quito the most as claimed in claim 1 component nano composite material, it is characterised in that institute
State template and refer to there is fine graded porous structure and be provided that abundant carbon source is for preparing the natural biological material of porous carbon matrix
Material.
The preparation method of a kind of porous carbon Quito the most as claimed in claim 1 component nano composite material, it is characterised in that institute
State pretreatment to refer to: described template be placed in ethanol and carry out sonic oscillation or stir process, then cleaning is dried.
The preparation method of a kind of porous carbon Quito the most as claimed in claim 1 component nano composite material, it is characterised in that institute
State the first impregnation liquid and refer to that the inorganic salt solution of precious metal ion, described first impregnation liquid are concentration 0.05～0.5mmol/L
Ethanol solution or aqueous solution.
The preparation method of a kind of porous carbon Quito the most as claimed in claim 4 component nano composite material, it is characterised in that institute
State the combination of one or more that precious metal ion includes in palladium, platinum, gold, silver, copper.
The preparation method of a kind of porous carbon Quito the most as claimed in claim 1 component nano composite material, it is characterised in that institute
State the second impregnation liquid and refer to that the inorganic salt solution of transition metal ions, described second impregnation liquid are concentration 0.01～0.1mol/L
Ethanol solution or aqueous solution.
The preparation method of a kind of porous carbon Quito the most as claimed in claim 7 component nano composite material, it is characterised in that institute
The inorganic salt stating transition metal ions includes stannum, antimony, zinc, ferrum, cobalt, nickel, indium, the nitrate of cerium, hydrochlorate, sulfate, sulfuration
The combination of one or more in thing.
The preparation method of a kind of porous carbon Quito the most as claimed in claim 1 component nano composite material, it is characterised in that described
The atmosphere that atmosphere calcining uses refers to the mixed gas of air, nitrogen or oxygen and nitrogen.
The preparation method of a kind of porous carbon Quito the most as claimed in claim 8 component nano composite material, it is characterised in that described
In mixed gas, oxygen is 20:80～0:100 with the volume range of nitrogen.
The preparation method of a kind of porous carbon Quito the most as claimed in claim 1 component nano composite material, it is characterised in that institute
The calcine technology stating atmosphere calcining is: the heating rate of 1～10 DEG C rises to 400～700 DEG C and calcines.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108546962A (en) * | 2018-03-29 | 2018-09-18 | 上海大学 | A kind of preparation method of the electrolysis water oxygen-separating catalyst of high specific surface area porous carbon doped iridium |
| CN108878909A (en) * | 2018-07-13 | 2018-11-23 | 中南大学 | A kind of three-dimensional porous composite material and preparation method and application based on biomass |
| CN111161904A (en) * | 2020-01-04 | 2020-05-15 | 浙江大学 | Preparation method of light high-conductivity porous conductive agent and application of light high-conductivity porous conductive agent in battery electrode |
| CN111762770A (en) * | 2020-05-25 | 2020-10-13 | 浙江工业大学 | Preparation method of oxygen-containing functional group functionalized porous carbon spheres |
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| US20090304570A1 (en) * | 2006-12-08 | 2009-12-10 | Sang Ho Kim | Manufacturing methods of mesoporous carbon structure with spray drying or spray pyrolysis and composition thereof |
| CN101780952A (en) * | 2010-03-26 | 2010-07-21 | 上海交通大学 | Method for preparing loading functional oxide porous carbon |
| CN102716740A (en) * | 2012-06-12 | 2012-10-10 | 上海交通大学 | Method for preparing photocatalytic material with multi-component porous classification structure |
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2016
- 2016-08-11 CN CN201610657481.2A patent/CN106276856B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090304570A1 (en) * | 2006-12-08 | 2009-12-10 | Sang Ho Kim | Manufacturing methods of mesoporous carbon structure with spray drying or spray pyrolysis and composition thereof |
| CN101249952A (en) * | 2008-03-27 | 2008-08-27 | 上海交通大学 | Method for preparing self-doping nitrogen grading porous oxide by using biomass template |
| CN101780952A (en) * | 2010-03-26 | 2010-07-21 | 上海交通大学 | Method for preparing loading functional oxide porous carbon |
| CN102716740A (en) * | 2012-06-12 | 2012-10-10 | 上海交通大学 | Method for preparing photocatalytic material with multi-component porous classification structure |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108546962A (en) * | 2018-03-29 | 2018-09-18 | 上海大学 | A kind of preparation method of the electrolysis water oxygen-separating catalyst of high specific surface area porous carbon doped iridium |
| CN108546962B (en) * | 2018-03-29 | 2020-01-17 | 上海大学 | Preparation method of high-specific-surface-area porous carbon iridium-doped electrolyzed water oxygen evolution catalyst |
| CN108878909A (en) * | 2018-07-13 | 2018-11-23 | 中南大学 | A kind of three-dimensional porous composite material and preparation method and application based on biomass |
| CN111161904A (en) * | 2020-01-04 | 2020-05-15 | 浙江大学 | Preparation method of light high-conductivity porous conductive agent and application of light high-conductivity porous conductive agent in battery electrode |
| CN111762770A (en) * | 2020-05-25 | 2020-10-13 | 浙江工业大学 | Preparation method of oxygen-containing functional group functionalized porous carbon spheres |
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