CN107602928A - A kind of preparation method of nitrogen-doped nanometer cellulose/carbon nano-fiber composite material - Google Patents
A kind of preparation method of nitrogen-doped nanometer cellulose/carbon nano-fiber composite material Download PDFInfo
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- CN107602928A CN107602928A CN201710793747.0A CN201710793747A CN107602928A CN 107602928 A CN107602928 A CN 107602928A CN 201710793747 A CN201710793747 A CN 201710793747A CN 107602928 A CN107602928 A CN 107602928A
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Abstract
The present invention relates to a kind of preparation method of nitrogen-doped nanometer cellulose/carbon nano-fiber composite material, belong to field of nanocomposite materials.The present invention destroys coconut palm petiole structure by Steam explosion treatment, hydrolyzed hemicellulose, lignin etc., cleaned again through dissolving, high intensity is made, high elastic modulus, the good coconut palm petiole nano-cellulose of translucency, the radius of nitrogen-atoms is recycled to be approached with carbon atom, it is easily accessible the characteristics of CNT lattice forms C N keys, a large amount of patterns and the more uniform nitrogen-doped carbon nanometer pipe of size are generated by Gaseous Detonation, change CNT local charge density using N doping, improve the electron transmission of CNT, reduce resistance coefficient, because the nitrogen-containing functional group that N doping introduces can bring quasi- Faraday effect, effectively improve the specific capacity of carbon nano-tube super-capacitor, it is made and has high intensity and the nano composite material of excellent conductive performance concurrently, it can be applied to lithium ion battery, the fields such as ultracapacitor.
Description
Technical field
The present invention relates to a kind of preparation method of nitrogen-doped nanometer cellulose/carbon nano-fiber composite material, belong to nanometer
Technical field of composite materials.
Background technology
Biomass nano material element is developed from biomass material, and functional product is prepared with this and can further improve biology
The added value and utilization ratio of matter raw material.Biomass resource includes various natural resources and its derives from resource, is distributed on earth
Extensively, there is recyclability, it is inexhaustible.Cellulose is that the day most wide, reserves are most abundant is distributed in nature
Right high polymer material, be mainly derived from the cell membrane of higher plant and timber, as cotton content of cellulose almost be up to 100%,
The content of cellulose of timber is in 40-50% or so, agricultural waste material（Soybean peel, stalk, bagasse）And cellulose is important
Source.Cellulose is in industrial circle as the additive of weaving, paper and paper pulp, food and pharmaceutical industry has huge exploitation should
Use potentiality.
For carbon fiber by organic fiber or asphaltic base raw material through being carbonized and being obtained after graphitization processing, its phosphorus content is high
In 85%, it can be used as the reinforcing fiber of composite.In recent years, researcher is by improving the preparation technology of carbon fiber, with reference to elder generation
The analysis means entered, realize the structure control of carbon fiber.The research trend of carbon fiber just towards high-performance, high function and it is low into
The direction of this change is developed.
Nanometer technology is the new and high technology developed in the world since last decade, as a kind of emerging excellent performance
Material, application prospect is considerable.In the resourceful area of the cocos such as Hainan, Guangdong, it is coming off naturally, have it is slight
The coconut tree branches and leaves of anti-corrosion function are seen everywhere, and have a strong impact on traffic safety and the city appearance of the city.Relevant agricultural wastes coconut palm petiole
It is seldom that the research of recycling and high-valued application discloses report.Cellulose is extracted from coconut palm petiole and as preparation Nanowire
The raw material of element is tieed up, is advantageous to changing rejected material to useful resource and Efficient Cycle utilizes, meet the policy of national sustainable development, have good
Environmental benefit.Cellulose is extracted from coconut palm petiole, prepares the good nano-cellulose of high intensity, high elastic modulus, translucency
（Cellulose nanofibers, CellNF）With electric conductivity is good, carbon nano-fiber of high intensity（Carbon
Nanofibers, CNF）, and two kinds of materials progress are compound, prepare the nano combined material for having high intensity and excellent conductive performance concurrently
Material, can be applied to the fields such as lithium ion battery, ultracapacitor.
The content of the invention
The technical problems to be solved by the invention：Mainly added for current carbon fiber by materials such as coal tar, asphalt
Work is produced and obtained, and this kind of resource belongs to non-renewable resources, limits following development of carbon fiber, and template is wanted to template
Ask very high, production cost is high, and the yield of chemical vapor deposition for carbon nanotubes is high, but its experimental procedure is more complicated, instead
Answer condition harsh, the problems such as caliber is whard to control provides a kind of nitrogen-doped nanometer cellulose/carbon nano-fiber composite material
Preparation method.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of preparation method of nitrogen-doped nanometer cellulose/carbon nano-fiber composite material, it is characterised in that specific preparation process
For：
（1）Crushed after the washing of coconut palm petiole is air-dried, cross 40 mesh sieves, obtain coconut palm petiole powder；
（2）Take coconut palm petiole powder to be fitted into Steam explosion treatment in steam blasting tank, obtain Steam explosion treatment coconut palm petiole powder；
（3）Steam explosion treatment coconut palm petiole powder is immersed in 1~2h of reaction in hydrogenperoxide steam generator, then uses sodium hydroxide solution
It is 10~11 to adjust pH, continues 1~2h of reaction, filters to obtain filter residue, filter residue alcohol is washed into drying, obtains coconut palm petiole nano-cellulose；
（4）Take ferrocene to be fitted into coconut palm petiole nano-cellulose in Gaseous Detonation pipe, ammonia and oxygen are re-filled with, after being filled with
Sealing gas phase Detonation Tube simultaneously heats, recycling high-energy igniter generation electric spark ignition gas, gas in discharge pipe after 5~10min
Body, product is collected, obtains nitrogen-doped nanometer cellulose/carbon nano-fiber composite material.
Step（2）The Steam explosion treatment is heated to 110~120 for coconut palm petiole powder is fitted into steam blasting tank
DEG C, and it is 1.5~2.5MPa to be passed through vapor to pressure inside the tank into steam blasting tank, after keeping 5~8min of pressure, opens and steams
Tank valve pressure release is broken in steam explosion, coconut palm petiole powder is taken out after pressure release to normal pressure, and washed 3~5 times with 60~80 DEG C of deionized waters.
Step（3）The hydrogenperoxide steam generator mass fraction is 10%, and dosage is Steam explosion treatment coconut palm petiole powder quality
10 times, reaction temperature is 60~80 DEG C of waters bath with thermostatic control.
Step（3）The sodium hydroxide solution mass fraction is 5%, and reaction temperature is 80~90 DEG C of waters bath with thermostatic control.
Step（4）The mass ratio of the ferrocene and coconut palm petiole nano-cellulose is 1：30.
Step（4）Ammonia and the oxygen volume ratio is 1：3~1：4.
Step（4）Initial evacuation is filled with ammonia and oxygen to gas phase to 0.08~0.09MPa in the Gaseous Detonation pipe
Detonation overpressure is 0.15~0.25MPa, and gas phase Detonation Tube is sealed after being filled with and is heated to 150~180 DEG C.
Compared with other method, advantageous effects are the present invention：
The present invention destroys coconut palm petiole structure, hydrolyzed hemicellulose, lignin etc. by Steam explosion treatment, then is cleaned through dissolving,
The good coconut palm petiole nano-cellulose of high intensity, high elastic modulus, translucency is made, recycles the radius and carbon atom of nitrogen-atoms
It is close, the characteristics of CNT lattice forms C-N keys is easily accessible, a large amount of patterns are generated by Gaseous Detonation and size is more equal
Even nitrogen-doped carbon nanometer pipe, change CNT local charge density using N doping, improve the electron transmission of CNT
Property, resistance coefficient is reduced, because the nitrogen-containing functional group that N doping introduces can bring quasi- Faraday effect, effectively improves carbon nanometer
The specific capacity of pipe ultracapacitor, be made have high intensity and the nano composite material of excellent conductive performance concurrently, can be applied to lithium from
The fields such as sub- battery, ultracapacitor.
Embodiment
Take coconut palm petiole that clean rear natural air drying is washed with deionized, be reloaded into pulverizer and crush, cross 40 mesh sieves, obtain coconut palm
Petiole powder, take 3~5kg coconut palm petiole powder to be fitted into steam blasting tank, be heated to 110~120 DEG C, and into steam blasting tank
It is 1.5~2.5MPa to be passed through vapor to pressure inside the tank, after keeping 5~8min of pressure, opens steam blasting tank valve pressure release, lets out
Coconut palm petiole powder is taken out after being depressed into normal pressure, and is washed 3~5 times with 60~80 DEG C of deionized waters, obtains Steam explosion treatment coconut palm petiole
Powder, 300~500g Steam explosion treatment coconut palm petiole powder is taken, it is 10% hydrogenperoxide steam generator to be immersed in 3~5L mass fractions
In, under 60~80 DEG C of waters bath with thermostatic control react 1~2h, then with mass fraction be 5% sodium hydroxide solution regulation pH be 10~11,
Continue 1~2h of reaction under 80~90 DEG C of waters bath with thermostatic control, filter to obtain filter residue, and washed with absolute ethyl alcohol during filter residue is in cleaning solution
Property, then be transferred in drying box, dried at 105~110 DEG C to constant weight, obtain coconut palm petiole nano-cellulose,
1~2g ferrocene and 30~60g coconut palm petiole nano-celluloses is taken to be fitted into Gaseous Detonation pipe, and it is evacuated to 0.08~
0.09MPa, then by volume 1：3~1：4 to be filled with ammonia and oxygen to Gaseous Detonation overpressure be 0.15~0.25MPa, is filled
Gas phase Detonation Tube is sealed after entering and is heated to 150~180 DEG C, recycles high-energy igniter to produce electric spark and ignites gas,
Stop heating, gas in discharge pipe, collects product, obtain nitrogen-doped nanometer cellulose/carbon nano-fiber composite wood after 5~10min
Material.
Example 1
Take coconut palm petiole that clean rear natural air drying is washed with deionized, be reloaded into pulverizer and crush, cross 40 mesh sieves, obtain coconut palm petiole
Powder, take 3kg coconut palm petiole powder to be fitted into steam blasting tank, be heated to 110 DEG C, and vapor is passed through extremely into steam blasting tank
Pressure inside the tank is 1.5MPa, after keeping pressure 5min, opens steam blasting tank valve pressure release, coconut palm petiole is taken out after pressure release to normal pressure
Powder, and washed 3 times with 60 DEG C of deionized waters, Steam explosion treatment coconut palm petiole powder is obtained, takes 300g Steam explosion treatment coconut palm leaves
Handle powder, it is immersed in 3L mass fractions and divides in 10% hydrogenperoxide steam generator, to react 1h under 60 DEG C of waters bath with thermostatic control, then with quality
It is 10 that number adjusts pH for 5% sodium hydroxide solution, continues to react 1h under 80 DEG C of waters bath with thermostatic control, filters to obtain filter residue, and with anhydrous second
Alcohol washs filter residue to cleaning solution in neutrality, then is transferred in drying box, is dried at 105 DEG C to constant weight, obtains coconut palm petiole nanofiber
Element, take 1g ferrocene to be fitted into 30g coconut palm petiole nano-celluloses in Gaseous Detonation pipe, and be evacuated to 0.08MPa, then by volume
Than 1：3 to be filled with ammonia and oxygen to Gaseous Detonation overpressure be 0.15MPa, and gas phase Detonation Tube is sealed after being filled with and is heated
To 150 DEG C, recycle high-energy igniter to produce electric spark and ignite gas, stop heating, gas in discharge pipe, collects production after 5min
Thing, obtain nitrogen-doped nanometer cellulose/carbon nano-fiber composite material.
Example 2
Take coconut palm petiole that clean rear natural air drying is washed with deionized, be reloaded into pulverizer and crush, cross 40 mesh sieves, obtain coconut palm petiole
Powder, take 4kg coconut palm petiole powder to be fitted into steam blasting tank, be heated to 115 DEG C, and vapor is passed through extremely into steam blasting tank
Pressure inside the tank is 2.0MPa, after keeping pressure 6min, opens steam blasting tank valve pressure release, coconut palm petiole is taken out after pressure release to normal pressure
Powder, and washed 4 times with 70 DEG C of deionized waters, Steam explosion treatment coconut palm petiole powder is obtained, takes 400g Steam explosion treatment coconut palm leaves
Handle powder, 4L mass fractions are immersed in 10% hydrogenperoxide steam generator, 1.5h to be reacted under 70 DEG C of waters bath with thermostatic control, then use quality
Fraction is that 5% sodium hydroxide solution regulation pH is 10, continues to react 1.5h under 85 DEG C of waters bath with thermostatic control, filters to obtain filter residue, and use nothing
Water-ethanol washs filter residue to cleaning solution in neutrality, then is transferred in drying box, is dried at 108 DEG C to constant weight, obtains coconut palm petiole nanometer
Cellulose, take 1g ferrocene to be fitted into 50g coconut palm petiole nano-celluloses in Gaseous Detonation pipe, and be evacuated to 0.08MPa, then press
Volume ratio 1：3 to be filled with ammonia and oxygen to Gaseous Detonation overpressure be 0.20MPa, and gas phase Detonation Tube is sealed simultaneously after being filled with
160 DEG C are heated to, recycles high-energy igniter to produce electric spark and ignites gas, stop heating, gas in discharge pipe, is received after 8min
Collect product, obtain nitrogen-doped nanometer cellulose/carbon nano-fiber composite material.
Example 3
Take coconut palm petiole that clean rear natural air drying is washed with deionized, be reloaded into pulverizer and crush, cross 40 mesh sieves, obtain coconut palm petiole
Powder, take 5kg coconut palm petiole powder to be fitted into steam blasting tank, be heated to 120 DEG C, and vapor is passed through extremely into steam blasting tank
Pressure inside the tank is 2.5MPa, after keeping pressure 8min, opens steam blasting tank valve pressure release, coconut palm petiole is taken out after pressure release to normal pressure
Powder, and washed 5 times with 80 DEG C of deionized waters, Steam explosion treatment coconut palm petiole powder is obtained, takes 500g Steam explosion treatment coconut palm leaves
Handle powder, it is immersed in 5L mass fractions and divides in 10% hydrogenperoxide steam generator, to react 2h under 80 DEG C of waters bath with thermostatic control, then with quality
It is 11 that number adjusts pH for 5% sodium hydroxide solution, continues to react 2h under 90 DEG C of waters bath with thermostatic control, filters to obtain filter residue, and with anhydrous second
Alcohol washs filter residue to cleaning solution in neutrality, then is transferred in drying box, is dried at 110 DEG C to constant weight, obtains coconut palm petiole nanofiber
Element, take 2g ferrocene to be fitted into 60g coconut palm petiole nano-celluloses in Gaseous Detonation pipe, and be evacuated to 0.09MPa, then by volume
Than 1：4 to be filled with ammonia and oxygen to Gaseous Detonation overpressure be 0.25MPa, and gas phase Detonation Tube is sealed after being filled with and is heated
To 180 DEG C, recycle high-energy igniter to produce electric spark and ignite gas, stop heating, gas in discharge pipe, is collected after 10min
Product, obtain nitrogen-doped nanometer cellulose/carbon nano-fiber composite material.
Reference examples：The carbon nano-tube fibre of Beijing new material company production.
This experiment is on the basis of the nano-cellulose base carbon nano-fiber prepared, then the coconut palm petiole nanometer with preparation
Cellulose carries out compound, obtained coconut palm petiole nano-cellulose/carbon nano-fiber flexible conductive film.
The composite membrane of example and reference examples is detected, specific detection is as follows：
Tensile property is tested：Composite membrane A, B, C are cut into long 35mm, wide 5mm batten respectively（Batten thickness about 0.065mm）.
Batten is stretched using omnipotent mechanics machine, specimen holder ensures the effective length of batten in 25 mm between two fixtures
Left and right, use 1000N sensor, loading velocity 1mm/min.All samples measurement is at least repeated 3 times, and calculates its Young
The average value of modulus and tensile strength.
Electrical performance testing：Utilize RTS-8 type four-point probes（Chinese four probe scientific ＆ technical corporation）To composite membrane A, B, C
Electric conductivity tested, composite film thickness about 0.065mm, diameter 38.5mm, instrument can calculate the electricity of composite membrane automatically
Conductance.
Specific testing result such as table 1.
Table 1
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| Tensile strength（MPa） | 66.7 | 65.1 | 67.8 | 61.2 |
| Electrical conductivity（s/cm） | 175.8 | 175.6 | 180.3 | 170.5 |
As shown in Table 1, the carbon nano-fiber that prepared by the present invention has good tensile property and good electric conductivity, can also be with it
His Material cladding, prepares electrode of ultracapacitor or lithium ion battery etc..
Claims (7)
1. a kind of preparation method of nitrogen-doped nanometer cellulose/carbon nano-fiber composite material, it is characterised in that specific to prepare step
Suddenly it is：
（1）Crushed after the washing of coconut palm petiole is air-dried, cross 40 mesh sieves, obtain coconut palm petiole powder；
（2）Take coconut palm petiole powder to be fitted into Steam explosion treatment in steam blasting tank, obtain Steam explosion treatment coconut palm petiole powder；
（3）Steam explosion treatment coconut palm petiole powder is immersed in 1~2h of reaction in hydrogenperoxide steam generator, then uses sodium hydroxide solution
It is 10~11 to adjust pH, continues 1~2h of reaction, filters to obtain filter residue, filter residue alcohol is washed into drying, obtains coconut palm petiole nano-cellulose；
（4）Take ferrocene to be fitted into coconut palm petiole nano-cellulose in Gaseous Detonation pipe, ammonia and oxygen are re-filled with, after being filled with
Sealing gas phase Detonation Tube simultaneously heats, recycling high-energy igniter generation electric spark ignition gas, gas in discharge pipe after 5~10min
Body, product is collected, obtains nitrogen-doped nanometer cellulose/carbon nano-fiber composite material.
2. a kind of preparation method of nitrogen-doped nanometer cellulose/carbon nano-fiber composite material as claimed in claim 1, it is special
Sign is, step（2）The Steam explosion treatment is heated to 110~120 for coconut palm petiole powder is fitted into steam blasting tank
DEG C, and it is 1.5~2.5MPa to be passed through vapor to pressure inside the tank into steam blasting tank, after keeping 5~8min of pressure, opens and steams
Tank valve pressure release is broken in steam explosion, coconut palm petiole powder is taken out after pressure release to normal pressure, and washed 3~5 times with 60~80 DEG C of deionized waters.
3. a kind of preparation method of nitrogen-doped nanometer cellulose/carbon nano-fiber composite material as claimed in claim 1, it is special
Sign is, step（3）The hydrogenperoxide steam generator mass fraction is 10%, and dosage is Steam explosion treatment coconut palm petiole powder quality
10 times, reaction temperature is 60~80 DEG C of waters bath with thermostatic control.
4. a kind of preparation method of nitrogen-doped nanometer cellulose/carbon nano-fiber composite material as claimed in claim 1, it is special
Sign is, step（3）The sodium hydroxide solution mass fraction is 5%, and reaction temperature is 80~90 DEG C of waters bath with thermostatic control.
5. a kind of preparation method of nitrogen-doped nanometer cellulose/carbon nano-fiber composite material as claimed in claim 1, it is special
Sign is, step（4）The mass ratio of the ferrocene and coconut palm petiole nano-cellulose is 1：30.
6. a kind of preparation method of nitrogen-doped nanometer cellulose/carbon nano-fiber composite material as claimed in claim 1, it is special
Sign is, step（4）Ammonia and the oxygen volume ratio is 1：3~1：4.
7. a kind of preparation method of nitrogen-doped nanometer cellulose/carbon nano-fiber composite material as claimed in claim 1, it is special
Sign is, step（4）Initial evacuation is filled with ammonia and oxygen to gas phase to 0.08~0.09MPa in the Gaseous Detonation pipe
Detonation overpressure is 0.15~0.25MPa, and gas phase Detonation Tube is sealed after being filled with and is heated to 150~180 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108872011A (en) * | 2018-06-26 | 2018-11-23 | 北京航空航天大学 | Alkali metal atom vapour density measurement method and measuring device based on coherent detection |
| CN109767927A (en) * | 2019-01-17 | 2019-05-17 | 中南大学 | A kind of preparation method of the supercapacitor biomass porous carbon of high-performance N doping |
| CN112522988A (en) * | 2020-12-10 | 2021-03-19 | 江门市高力依科技实业有限公司 | Special efficient agent containing sulfur-doped nanocrystalline cellulose for papermaking and preparation method thereof |
| CN115079338A (en) * | 2022-07-08 | 2022-09-20 | 湖北工业大学 | Nitrogen-doped carbon nanotube micro-nano optical fiber and gas sensor comprising same |
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| CN108872011A (en) * | 2018-06-26 | 2018-11-23 | 北京航空航天大学 | Alkali metal atom vapour density measurement method and measuring device based on coherent detection |
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| CN112522988A (en) * | 2020-12-10 | 2021-03-19 | 江门市高力依科技实业有限公司 | Special efficient agent containing sulfur-doped nanocrystalline cellulose for papermaking and preparation method thereof |
| CN115079338A (en) * | 2022-07-08 | 2022-09-20 | 湖北工业大学 | Nitrogen-doped carbon nanotube micro-nano optical fiber and gas sensor comprising same |
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