CN107188156A - A kind of preparation method of lotus flower stem nitrogen-doped carbon nano material - Google Patents
A kind of preparation method of lotus flower stem nitrogen-doped carbon nano material Download PDFInfo
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- CN107188156A CN107188156A CN201710501592.9A CN201710501592A CN107188156A CN 107188156 A CN107188156 A CN 107188156A CN 201710501592 A CN201710501592 A CN 201710501592A CN 107188156 A CN107188156 A CN 107188156A
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- lotus flower
- flower stem
- carbon nano
- nano material
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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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
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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Abstract
The invention discloses a kind of preparation method of lotus flower stem nitrogen-doped carbon nano material.Comprise the following steps that：(1) wash clean, drying, grind into powder after lotus flower stem being gathered；(2) the lotus flower stem pulverized is added in urea liquid and impregnated, dipping is dried after terminating, and presoma is made；(3) presoma is placed in tubular type kiln roasting, obtains pre- carbonized product；(4) pre- carbonized product is added and dried after being impregnated in KOH solution, then high-temperature roasting processing；(5) product after high-temperature roasting is dried in HCl solution after impregnation process, washing to neutrality, obtains lotus flower stem nitrogen-doped carbon nano material.The beneficial effects of the present invention are：Lotus flower stem is used to prepare nitrogen-doped carbon nano material for presoma, lotus flower stem abundance, the process of preparation is simple, safe and reliable, environmentally safe, can carry out quantization production.
Description
Technical field
Present invention relates particularly to technical field of nano material, more particularly to a kind of lotus flower stem nitrogen-doped carbon nano material
Preparation method.
Background technology
The economic interests with the rapid development of economy, people covet and ignore the protection to the energy and environment, now
Cause the anxiety of the energy and the severe exacerbation of environment.In order to realize that the reformation of resource is utilized, sustainable development path, carbon material are walked
Discovery cause the concern of numerous scientists.Stability and the extensive utilization in energy circle that carbon material has, promote various countries
Science, which is returned home, researchs and develops the good method of cost ineffective fruit.The method that tradition prepares carbon material has many defects, while in system
The pollution of environment can be caused in standby process, the introducing of nitrogen-atoms the performance of carbon material can be effectively improved into, this is a lot
Report and document in refer to.
Lotus flower stem is Nelumbonaceae draft water very plant, and lotus, lotus etc. are also known as when ancient times.The diameter of lotus flower stem can grow into
60cm or so, lotus flower stem is green, has many spinules above, them are protect just as umbrella, and the surface of lotus flower stem has
The wax mastoid process structure of many Nano grades, if with electron microscope observation, with regard to the nanometer for having many structures similar can be seen
Grade particles.The distribution of lotus flower stem widely, not only in China, is all distributed on West Asia, North America, India and Japan and other places,
Source widely, a kind of industrial crops is used as in Chinese many people.
There are some defects in face of the existing method for preparing carbon material, production cost is higher, and reaction condition is more harsh, react
Cycle is long, and raw material are not enough, and cost is too high.The yield of lotus flower stem is also considerable, and some lotus flower stems are as fuel or waste
It is thrown away or burns up, not only cause environmental pollution, will also result in a certain degree of wasting of resources, therefore be used for from lotus flower stem
The research of carbon material, is conducive to improving its added value, for environmental protection and increasing economic efficiency with important double-deck benefit.
The content of the invention
It is an object of the invention to provide a kind of biomass using lotus flower stem as raw material, to prepare a kind of nanometer of nitrogen-doped carbon
Material, a kind of cheap, simple new method of preparation process is provided for the preparation of carbon material.This method abundant raw material, raw material is more
Cheap and wide material sources, can realize quantization production, effectively save industry cost.
The technical proposal of the invention is realized in this way.
The present invention provides a kind of preparation method of lotus flower stem nitrogen-doped carbon nano material, comprises the following steps that：
(1) wash clean after lotus flower stem being gathered, dry, grind into powder；
(2) the lotus flower stem pulverized is added in urea liquid and impregnated, dried after dipping and presoma is made；
(3) presoma is placed in tubular type kiln roasting and obtains pre- carbonized product；Sintering temperature is 300 DEG C -800 DEG C, roasting
Time is 1~4h；
(4) pre- carbonized product is added in KOH solution and impregnated, etch pore-creating, dipping is dried after terminating；
(5) the pre- carbonized product that KOH impregnation process is crossed is placed in tubular type kiln roasting, sintering temperature is 600 DEG C -900 DEG C,
Roasting time is 1h-4h；
(6) impregnation process, washing in hydrochloric acid solution by the product after being calcined in step (5), removes hetero atom, and dry
It is dry, obtain lotus flower stem nitrogen-doped carbon nano material.
In the present invention, in step (1), the particle diameter pulverized is 12h-36h in the mesh of 50 mesh -200, drying time.
In the present invention, in step (2), the mass ratio of lotus flower stem and urea is 1:0.5-1:3；Dipping temperature is 20 DEG C -60
DEG C, dip time is 4h-24h.
In the present invention, in step (3), during roasting, heating rate is 5 DEG C/min-10 DEG C/min.
In the present invention, in step (3), sintering temperature is 300~500 DEG C.
In the present invention, in step (4), pre- carbonized product and KOH mass ratio is 1:1-1：3, the concentration of KOH solution is 1-
3mol/L。
In the present invention, in step (5), heating rate is 5 DEG C/min-10 DEG C/min.
In the present invention, in step (6), concentration of hydrochloric acid solution is 1-3mol/L, and dip time is 24h-48h.
Compared to the prior art, the beneficial effects of the present invention are：A kind of lotus flower stem nitrogen-doped carbon nanometer material of the present invention
The preparation method of material, uses lotus flower stem to prepare nitrogen-doped carbon nano material, lotus flower stem abundance, the process of preparation for presoma
Technique is simple, safe and reliable, environmentally safe, can carry out quantization production, life can be effectively reduced compared with traditional carbon source
Produce cost.
Brief description of the drawings
Fig. 1 is the TG curve maps of the lotus flower stem of embodiment 1.
Embodiment
Technical scheme is further described with reference to specific embodiment, but the present invention is not limited to
Following embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not under the premise of creative work is made
The other embodiment obtained, belongs to the scope of the present invention.
Embodiment 1
A kind of preparation method of lotus flower stem nitrogen-doped carbon nano material, specifically includes following steps：
(1) wash clean after lotus flower stem being gathered, 100 DEG C are dried in Muffle furnace, dry 12h, are ground after drying
Into particle diameter 100 mesh lotus flower stem powder；
(2) the preferred mass ratio of preparation urea liquid, lotus flower stem and urea is 1:3, the lotus flower stem pulverized is added
Impregnated in solution, dipping temperature is 20 DEG C, and dip time is 4h-24h, then in 30 DEG C of dry for standby, presoma is made；
(3) presoma being placed in tube furnace and be calcined under nitrogen protection, roasting time is 1h, heating rate is 8 DEG C/
Min, sintering temperature is 500 DEG C, that is, obtains the product of pre- carbonization, then Temperature fall；
(4) KOH solution is prepared, the preferred mass ratio of pre- carbonized product and KOH is 1:1, KOH solution concentration is 1M, will be pre-
Carbonized product, which is added in solution, to be impregnated, and dip time is 4h-24h, then in 30 DEG C of dry for standby；
(5) the KOH pre- carbonized products treated are placed in tube furnace, are calcined under nitrogen protection, roasting time is 1h,
Heating rate is 8 DEG C/min, and sintering temperature is 600 DEG C, then Temperature fall；
(6) hydrochloric acid solution is prepared, concentration of hydrochloric acid solution is 1M, and dip time is 24h, and drying temperature is 60 DEG C, during drying
Between be 36h, to after high-temperature roasting product carry out impregnation process, wash to neutrality dry for standby with ethanol and deionized water,
Obtain lotus flower stem nitrogen-doped carbon nano material.
Fig. 1 is the TG curve maps of the lotus flower stem of embodiment 1, and we can determine whether go out the preliminary carbonisation of lotus flower stem from figure
Temperature.
Embodiment 2
A kind of preparation method of lotus flower stem nitrogen-doped carbon nano material, specifically includes following steps：
(1) wash clean after lotus flower stem being gathered, 100 DEG C are dried in Muffle furnace, dry 12h, are ground after drying
Into particle diameter 100 mesh lotus flower stem powder；
(2) the preferred mass ratio of preparation urea liquid, lotus flower stem and urea is 1:2, the lotus flower stem pulverized is added
Impregnated in solution, dipping temperature is 60 DEG C, and dip time is 24h, then in 100 DEG C of dry for standby, presoma is made；
(3) presoma being placed in tube furnace and be calcined under nitrogen protection, roasting time is 1h, heating rate is 8 DEG C/
Min, sintering temperature is 500 DEG C, that is, obtains the product of pre- carbonization, then Temperature fall；
(4) KOH solution is prepared, the preferred mass ratio of pre- carbonized product and KOH is 1:2, KOH solution concentration is 1M, will be pre-
Carbonized product, which is added in solution, to be impregnated, and dip time is 24h, then in 100 DEG C of dry for standby；
(5) the KOH pre- carbonized products treated are placed in tube furnace, are calcined under nitrogen protection, roasting time is 1h,
Heating rate is 8 DEG C/min, and sintering temperature is 700 DEG C, then Temperature fall；
(6) hydrochloric acid solution is prepared, concentration of hydrochloric acid solution is 1M, and dip time is 24h, and drying temperature is 60 DEG C, during drying
Between be 36h, to after high-temperature roasting product carry out impregnation process, wash to neutrality dry for standby with ethanol and deionized water,
Obtain lotus flower stem nitrogen-doped carbon nano material.
Embodiment 3
A kind of preparation method of lotus flower stem nitrogen-doped carbon nano material, specifically includes following steps：
(1) wash clean after lotus flower stem being gathered, 100 DEG C are dried in Muffle furnace, dry 12h, are ground after drying
Into particle diameter 100 mesh lotus flower stem powder；
(2) the preferred mass ratio of preparation urea liquid, lotus flower stem and urea is 1:1, the lotus flower stem pulverized is added
Impregnated in solution, dipping temperature is 20 DEG C, and dip time is 24h, then in 30 DEG C of -200 DEG C of dry for standby, presoma is made；
(3) presoma being placed in tube furnace and be calcined under nitrogen protection, roasting time is 1h, heating rate is 8 DEG C/
Min, sintering temperature is 500 DEG C, that is, obtains the product of pre- carbonization, then Temperature fall；
(4) KOH solution is prepared, the preferred mass ratio of pre- carbonized product and KOH is 1:1, KOH solution concentration is 1M, will be pre-
Carbonized product, which is added in solution, to be impregnated, and dip time is 24h, then in 100 DEG C of dry for standby；
(5) the KOH pre- carbonized products treated are placed in tube furnace, are calcined under nitrogen protection, roasting time is 1h,
Heating rate is 8 DEG C/min, and sintering temperature is 800 DEG C, then Temperature fall；
(6) hydrochloric acid solution is prepared, concentration of hydrochloric acid solution is 1M, and dip time is 24h, and drying temperature is 60 DEG C, during drying
Between be 36h, to after high-temperature roasting product carry out impregnation process, wash to neutrality dry for standby with ethanol and deionized water,
Obtain lotus flower stem nitrogen-doped carbon nano material.
Embodiment 4
A kind of preparation method of lotus flower stem nitrogen-doped carbon nano material, specifically includes following steps：
(1) wash clean after lotus flower stem being gathered, 100 DEG C are dried in Muffle furnace, dry 12h, are ground after drying
Into particle diameter 100 mesh lotus flower stem powder；
(2) the preferred mass ratio of preparation urea liquid, lotus flower stem and urea is 1:3, the lotus flower stem pulverized is added
Impregnated in solution, dipping temperature is 20 DEG C, and dip time is 4h-24h, then in 100 DEG C of dry for standby, presoma is made；
(3) presoma being placed in tube furnace and be calcined under nitrogen protection, roasting time is 1h, heating rate is 8 DEG C/
Min, sintering temperature is 500 DEG C, that is, obtains the product of pre- carbonization, then Temperature fall；
(4) KOH solution is prepared, the preferred mass ratio of pre- carbonized product and KOH is 1:2, KOH solution concentration is 1M, will be pre-
Carbonized product, which is added in solution, to be impregnated, and dip time is 24h, then in 200 DEG C of dry for standby；
(5) the KOH pre- carbonized products treated are placed in tube furnace, are calcined under nitrogen protection, roasting time is 1h,
Heating rate is 8 DEG C/min, and sintering temperature is 900 DEG C, then Temperature fall；
(6) hydrochloric acid solution is prepared, concentration of hydrochloric acid solution is 1M, and dip time is 24h, and drying temperature is 60 DEG C, during drying
Between be 36h, to after high-temperature roasting product carry out impregnation process, wash to neutrality dry for standby with ethanol and deionized water,
Obtain lotus flower stem nitrogen-doped carbon nano material.
Embodiment 5
A kind of preparation method of lotus flower stem nitrogen-doped carbon nano material, specifically includes following steps：
(1) wash clean after lotus flower stem being gathered, 100 DEG C are dried in Muffle furnace, dry 12h, are ground after drying
Into particle diameter 100 mesh lotus flower stem powder；
(2) the preferred mass ratio of preparation urea liquid, lotus flower stem and urea is 1:2, the lotus flower stem pulverized is added
Impregnated in solution, dipping temperature is 20 DEG C, and dip time is 24h, then in 100 DEG C of dry for standby, presoma is made；
(3) presoma being placed in tube furnace and be calcined under nitrogen protection, roasting time is 3h, heating rate is 5 DEG C/
Min, sintering temperature is 500 DEG C, that is, obtains the product of pre- carbonization, then Temperature fall；
(4) KOH solution is prepared, the preferred mass ratio of pre- carbonized product and KOH is 1:1, KOH solution concentration is 1M, will be pre-
Carbonized product, which is added in solution, to be impregnated, and dip time is 4h-24h, then in 100 DEG C of dry for standby；
(5) the KOH pre- carbonized products treated are placed in tube furnace, are calcined under nitrogen protection, roasting time is 3h,
Heating rate is 8 DEG C/min, and sintering temperature is 1000 DEG C, then Temperature fall；
(6) hydrochloric acid solution is prepared, concentration of hydrochloric acid solution is 1M, and dip time is 24h, and drying temperature is 60 DEG C, during drying
Between be 36h, to after high-temperature roasting product carry out impregnation process, wash to neutrality dry for standby with ethanol and deionized water,
Obtain lotus flower stem nitrogen-doped carbon nano material.
The above is only the basic explanation under present inventive concept, and according to technical scheme done it is any etc.
Effect conversion, all should belong to protection scope of the present invention.
Claims (8)
1. a kind of preparation method of lotus flower stem nitrogen-doped carbon nano material, it is characterised in that comprise the following steps that：
(1) wash clean after lotus flower stem being gathered, dry, grind into powder；
(2) the lotus flower stem pulverized is added in urea liquid and impregnated, dried after dipping and presoma is made；
(3) presoma is placed in tubular type kiln roasting and obtains pre- carbonized product；Sintering temperature is 300 DEG C -800 DEG C, roasting time
For 1~4h；
(4) pre- carbonized product is added in KOH solution and impregnated, dipping is dried after terminating；
(5) the pre- carbonized product that KOH impregnation process is crossed is placed in tubular type kiln roasting, sintering temperature is 600 DEG C -900 DEG C, roasting
Time is 1h-4h；
(6) by the product after being calcined in step (5) in hydrochloric acid solution impregnation process, be washed out and dry, obtain lotus flower stem
Nitrogen-doped carbon nano material.
2. the preparation method of lotus flower stem nitrogen-doped carbon nano material according to claim 1, it is characterised in that：Step (1)
In, drying time is 12h-36h, and the particle diameter pulverized is in the mesh of 50 mesh -200.
3. the preparation method of lotus flower stem nitrogen-doped carbon nano material according to claim 1, it is characterised in that step (2)
In, the mass ratio of lotus flower stem and urea is 1:0.5-1:3；Dipping temperature is 20 DEG C -60 DEG C, and dip time is 4h-24h.
4. the preparation method of lotus flower stem nitrogen-doped carbon nano material according to claim 1, it is characterised in that step (3)
In, during roasting, heating rate is 5 DEG C/min-10 DEG C/min.
5. the preparation method of lotus flower stem nitrogen-doped carbon nano material according to claim 1, it is characterised in that step (3)
In, sintering temperature is 300~500 DEG C.
6. the preparation method of lotus flower stem nitrogen-doped carbon nano material according to claim 1, it is characterised in that step (4)
In, the mass ratio of pre- carbonized product and KOH is 1:1-1：3, the concentration of KOH solution is 1-3mol/L.
7. the preparation method of lotus flower stem nitrogen-doped carbon nano material according to claim 1, it is characterised in that：Step (5)
In, heating rate is 5 DEG C/min-10 DEG C/min.
8. the preparation method of lotus flower stem nitrogen-doped carbon nano material according to claim 1, it is characterised in that：Step (6)
In, the concentration of hydrochloric acid solution is 1-3mol/L, and dip time is 24h-48h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114335530A (en) * | 2021-12-08 | 2022-04-12 | 山东精工电子科技有限公司 | Carbon-coated ternary electrode material prepared from lotus rhizome and application thereof |
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| CN105731447A (en) * | 2016-04-27 | 2016-07-06 | 华中科技大学 | Preparation method of three-dimensional hierarchical porous nitrogen-doped graphene and product |
| CN106365144A (en) * | 2016-08-31 | 2017-02-01 | 青岛大学 | Method for preparing lotus leaf carbon nanometer material |
| CN106532026A (en) * | 2016-12-19 | 2017-03-22 | 中国科学院山西煤炭化学研究所 | Sulfur-activated carbon/graphene composite material and application thereof |
| CN106744788A (en) * | 2016-11-14 | 2017-05-31 | 天津工业大学 | The preparation method of biomass-based N doping three-dimensional multistage hole carbon material |
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2017
- 2017-06-27 CN CN201710501592.9A patent/CN107188156A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105731447A (en) * | 2016-04-27 | 2016-07-06 | 华中科技大学 | Preparation method of three-dimensional hierarchical porous nitrogen-doped graphene and product |
| CN106365144A (en) * | 2016-08-31 | 2017-02-01 | 青岛大学 | Method for preparing lotus leaf carbon nanometer material |
| CN106744788A (en) * | 2016-11-14 | 2017-05-31 | 天津工业大学 | The preparation method of biomass-based N doping three-dimensional multistage hole carbon material |
| CN106532026A (en) * | 2016-12-19 | 2017-03-22 | 中国科学院山西煤炭化学研究所 | Sulfur-activated carbon/graphene composite material and application thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114335530A (en) * | 2021-12-08 | 2022-04-12 | 山东精工电子科技有限公司 | Carbon-coated ternary electrode material prepared from lotus rhizome and application thereof |
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Application publication date: 20170922 |