CN109853086A - A kind of lignin/cellulose acetate base electrostatic spinning carbon fiber and the preparation method and application thereof - Google Patents
A kind of lignin/cellulose acetate base electrostatic spinning carbon fiber and the preparation method and application thereof Download PDFInfo
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- CN109853086A CN109853086A CN201811327706.3A CN201811327706A CN109853086A CN 109853086 A CN109853086 A CN 109853086A CN 201811327706 A CN201811327706 A CN 201811327706A CN 109853086 A CN109853086 A CN 109853086A
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Abstract
The invention discloses lignin/cellulose acetate base electrostatic spinning carbon fibers and its preparation method and application.In the presence of a catalyst being modified lignin and cellulose acetate using isocyanates bifunctional makes two macromolecular copolymerization, it obtains containing using cellulose acetate molecule as main chain, lignin molecule is the spinning solution of the macromolecular structure of side chain, precursor fibre is made by electrostatic spinning, then carbon fiber is made through pre-oxidation treatment and carbonization treatment.The present invention is linked together lignin and cellulose acetate by chemical modification, improves the uniformity and mobility of spinning solution, by modification during preparing spinning solution, realizes simple sustainable carbon fiber preparation.Carbon fiber made from the method for the present invention has good fibre morphology, high mechanicalness and absorption property, there is applications well prospect in terms of as electrode, reinforcing material and adsorbent, the full biomass base carbon fibre for production high quality, green, low cost provides guarantee.
Description
Technical field
The invention belongs to biological material processing technique fields, and in particular to a kind of lignin/cellulose acetate base electrostatic
Spinning carbon fiber and the preparation method and application thereof
Background technique
Problem of environmental pollution caused by increasingly depleted and fossil resource use with fossil energy, with fossil energy
The problem of shortage of resources of industry faces, how the environmentally protective reproducible biomass resource of significantly more efficient utilization goes to substitute
Fossil resource becomes the problem of urgent need to resolve.
Lignin is more than second natural polymer that cellulose is only second to existing for nature, has phosphorus content
Height, containing phenyl ring, the advantages that green is renewable.The recycling of progress thermal energy is gone mainly as paper pulp papermaking by-product at present, seldom
By further processing and utilization, the serious waste of resource is caused, or even serious pollution can be caused to environment.Lignin
Higher value application is target for a long time, and with the continuous improvement that people recognize energy crisis, this target becomes more
It is prominent.Lignin structure is complicated, containing phenyl ring, methoxyl group, phenol through many functional groups and chemical bonds such as base, Suo Ji and shuttle methyl,
So having very strong reactivity, the lignin that exists for of these groups carries out chemical modification, realizes that comprehensive utilization provides
Possibility, and the phosphorus content in lignin is up to 60%, therefore is considered as the suitable feedstock for preparing carbon material.
1860s, the clear male of the nearly rattan of Japanese has invented first manufactures carbon fiber with polyacrylonitrile fibre,
Afterwards by the continuous development of decades, and occur in succession using pitch, viscose fiber as the carbon fiber product of matrix.With petroleum
The worsening shortages of based raw material polyacrylonitrile develop renewable, the degradable new bio material carbon fiber of one kind and have become one kind
Inevitable trend.Environment can preferably be protected by preparing lignin base carbon fibre, increase the potential value of lignin, have good economy
Benefit.
Summary of the invention
The purpose of the present invention is to provide a kind of lignin/cellulose acetate base carbon fibre preparation method, party's legal systems
Standby obtained carbon fiber has good fibre morphology, high mechanicalness and high absorption property using full biomass raw material as substrate,
There is good application prospect in terms of as electrode and reinforcing material.
Technical scheme is as follows:
A kind of preparation method of lignin/cellulose acetate base electrostatic spinning carbon fiber will be wooden by electrospinning process
Quality/cellulose acetate base spinning solution is made carbon fiber precursor, then carbon fiber is made through pre-oxidation treatment and carbonization treatment,
In, by lignin and cellulose acetate in the presence of catalyst and difunctional isocyanates, carry out chemical modification reaction system
Obtain the lignin/cellulose acetate base spinning solution.
In the above-mentioned technical solutions, the difunctional isocyanates is isophorone diisocyanate, bis- isocyanide of MDI
Acid esters, 1,4- cyclohexane diisocyanate, TDI toluene di-isocyanate(TDI), 1,5- how diisocyanate, methylene diisocyanate
Ester, methyl -2,4- diisocyanate, dimer acid diisocyanate, methyl diphenylene diisocyanate, two isocyanide of xyxylene
One or more of acid esters.
In the above-mentioned technical solutions, the catalyst is dibutyl tin dilaurate, Dibutyltin oxide, stannous octoate
One of.
In the above-mentioned technical solutions, the reaction temperature of the chemical modification reaction is 60~100 DEG C, the reaction time 1
~10h.
In the above-mentioned technical solutions, in the chemical modification reaction, the lignin and cellulose acetate plus
Entering amount is 30:70~70:30 in mass ratio, the additional amount of the lignin and cellulose acetate be reaction solution quality 10~
30%.
In the above-mentioned technical solutions, in the chemical modification reaction, the difunctional isocyanates additional amount
It is the 2~20% of reaction solution quality, preferably 5~16%, more preferably 8~12%, the additional amount of the catalyst is anti-
Answer the 0.1~5% of liquid quality, preferably 0.5~3%, more preferably 1~3%.
In the above-mentioned technical solutions, in the chemical modification reaction, lignin and cellulose acetate are dissolved in solvent A
With the in the mixed solvent of solvent B, wherein the mixed proportion of solvent A and solvent B are 1~2:1 by volume, described molten as mixing
The solvent A of liquid/solvent B is acetone/N, N-dimethylformamide, glacial acetic acid/N, N-dimethylformamide, acetone/N, N dimethyl second
Amide or glacial acetic acid/N, N dimethyl acetamide.
In the above-mentioned technical solutions, in the electrospinning process, electrostatic potential is 15~35KV, receive distance for 10~
35cm, receiving rod revolving speed is 200~700r/min, and it is 0.1~1ml/h that spinning solution, which pushes away speed,.
In the above-mentioned technical solutions, the pre-oxidation treatment is to pre-oxidize carbon fiber precursor in air atmosphere,
Pre-oxidation by room temperature, be warming up to 200~300 DEG C with the rate of 0.01~2.00 DEG C/min, and at this temperature heat preservation 2~
10h obtains pre-oxidized fibers.
In the above-mentioned technical solutions, the carbonization treatment be will be through pre-oxidized fibers indifferent gas that pre-oxidation treatment obtains
Body protection is lower to heat carbonization treatment, is warming up to 600~1400 DEG C with 2~10 DEG C/min rate, and at this temperature heat preservation 2~
10h obtains lignin/cellulose acetate base electrostatic spinning carbon fiber.The inert gas is nitrogen, argon gas, one in helium
Kind.
In the present invention, the quality of above-mentioned reaction solution refers in chemical modification reaction, the reaction after each reactant is added
The gross mass of system, reaction solution carry out 1~10h of chemical modification reaction under suitable condition such as 60~100 DEG C of reaction temperature,
Lignin/cellulose acetate base the spinning solution is made.
The lignin being prepared the present invention also provides above-mentioned method/cellulose acetate base electrostatic spinning carbon fiber is being made
Application in standby adsorbent.The lignin that the method for the present invention obtains/cellulose acetate base electrostatic spinning carbon fiber has good
Absorption property can substitute the fine base carbon fibre of polypropylene and active carbon for adsorbing, such as adsorbing the absorption of methylene blue.
In the present invention, used lignin derives from biomass, such as includes that needlebush, leaf wood and non-timber are fine
The lignin isolated in dimension raw material, according to separation method difference can obtain wooden to be known as formic acid lignin, acetic acid wooden
Element and ethyl alcohol lignin etc..The isolated lignin of this means of different can be bought from the market, can also be voluntarily
It is prepared according to the document having disclosed.Present invention preferably employs ethyl alcohol lignin.Lignin of the present invention, preferably its point
Son amount is between 1000~50000.
In the present invention, cellulose acetate derives from the acetic acid anhydride modification of natural fiber.Cellulose acetate of the present invention, it is excellent
Select its acetyl content 37%~40%.
In the present invention, lignin and cellulose acetate are carried out using isocyanates bifunctional in the presence of a catalyst
Modified to make two macromolecular copolymerization to get to containing with cellulose acetate molecule main chain, lignin molecule is big point of side chain
The spinning solution of minor structure, spinning solution uniformly, good fluidity.Presoma fibre is made by electrostatic spinning in modified obtained spinning solution
Dimension, precursor fibre molecular weight is big, and molecular weight distribution is concentrated, good spinnability, and gained fiber is uniform.On the other hand, for wooden
Element and cellulose acetate are just handled during preparing spinning solution, and spinning solution is directly used in spinning, sustainable to go to make
Standby lignin/cellulose acetate base carbon fibre, overcomes current preparation method because precursor fibre prepares it well
The production post-processed afterwards without can be carried out carbon fiber serialization increases the problem of preparing energy consumption.Meanwhile method of the invention
The carbon fiber being prepared has good fibre morphology, high mechanicalness, good absorption property, as electrode and strengthening material
Material aspect has applications well prospect.
Carbon fiber of the invention prepares raw material not comprising any fossil feedstock, uses biomass material lignin and acetic acid
Cellulose is from a wealth of sources, price is cheap, is easy to regenerate, is environmentally protective as carbon fiber carbon usually source.
Detailed description of the invention
Fig. 1 is the figure of lignin/cellulose acetate base electrostatic spinning carbon fiber SEM made from the embodiment of the present invention 1.
Fig. 2 is lignin/cellulose acetate base electrostatic spinning carbon fiber methylene blue adsorption number made from the embodiment of the present invention 1
Effect picture.
Fig. 3 is lignin/cellulose acetate base electrostatic spinning mechanical properties of carbon fibre error made from the embodiment of the present invention 1
Analyze histogram.
Specific embodiment
Present invention will be described in further detail below with reference to the accompanying drawings and specific embodiments, but the present invention does not limit to
In these embodiments.In following embodiments, unless otherwise specified, used experimental method is conventional method, material used
Material, reagent etc. can be bought from biological or chemical company.
Following embodiment material therefors:
Ethyl alcohol lignin: digesting residue for corn stover, the preparation method is as follows: extracting corn stover using ethanol-water pulping method
Residue lignin is digested, concentration of alcohol 60%, solid-liquid ratio 1:10, Extracting temperature is 190 DEG C, extraction time 70min.It mentions
Aqueous precipitation after taking liquid to filter reconciles pH of mixed to 2 with hydrochloric acid hereinafter, precipitating for 24 hours, filters, and water-soluble with the hydrochloric acid of pH=2
Liquid rinses 3 to 5 times and obtains filter cake, and after filter cake is freeze-dried, grinding obtains ethyl alcohol lignin.
Cellulose acetate: Shanghai Aladdin biochemical technology limited liability company, model 9004-35-7, acetyl content
For 39.8wt%.
Electrostatic spinning machine: the micro-nano Science and Technology Ltd. of Shenzhen concerted effort, model TL-Pro.
Embodiment 1
It is prepared as follows ethyl alcohol lignin/cellulose acetate base electrostatic spinning carbon fiber:
(1) ethyl alcohol lignin and cellulose acetate are dissolved in acetone/N, N- dimethyl methyl according to mass ratio 50:50 (w/w)
The in the mixed solvent of amide (v/v:2:1) is separately added into two fourth of isophorone diisocyanate and tin dilaurate after being completely dissolved
Ji Xi, the final concentration of isophorone diisocyanate is respectively 0wt%, 2wt%, 4wt%, 6wt%, 8wt% in reaction solution,
The final concentration of 20wt% of the final concentration of 0.5wt% of dibutyl tin dilaurate, ethyl alcohol lignin and cellulose acetate, 60
72h is reacted at DEG C, obtains lignin/cellulose acetate base spinning solution；Chemically modified reaction, lignin and acetic acid in spinning solution
Cellulose links together, and forms using cellulose acetate molecule as main chain, and lignin molecule is the macromolecular structure of side chain；
(2) spinning solution that step (1) obtains is prepared into lignin/cellulose acetate base carbon fibre by electrospinning process
Precursor, the condition of electrostatic spinning are as follows: electrostatic pressure 25KV, receiving distance is 20cm, receives rod revolving speed 500r/min, spinning is molten
The fltting speed of liquid is 0.2mL/h；
(3) carbon fiber precursor obtained is placed in tube furnace, with the heating of 0.01 DEG C/min in air atmosphere
Rate is warming up to 200 DEG C, and keeps the temperature 720min and carry out pre-oxidation treatment；Then under nitrogen protection with the rate liter of 4 DEG C/min
Temperature keeps the temperature 120min and carries out heating carbonization treatment to 600 DEG C, obtains lignin/cellulose acetate base electrostatic spinning carbon fiber.
Carbon fiber electron microscope such as Fig. 1, Fig. 1 a~Fig. 1 ef obtained by embodiment respectively are isophorone diisocyanate and add
It is prepared when dosage 0wt% (CFs-1), 2wt% (CFs-2), 4wt% (CFs-3), 6wt% (CFs-4) and 8wt% (CFs-5)
Gained carbon fiber electron microscope.Fig. 1 is as it can be seen that gained carbon fiber hair when isophorone diisocyanate additive amount 0wt% or 2wt%
Raw adhesion phenomenon initially forms inhomogenous fiber when isophorone diisocyanate additive amount increases to 4wt%, and works as
When additive amount increases to 6wt%, continuous uniform fiber is generated, dosage is continued growing later, due to excessive gluing, leads
Fibre morphology is caused to be deteriorated.
Absorption property measurement is carried out as methylene blue adsorption number material.The adsorbent of 10mg is added to 100mL matter
It measures in the methylene blue solution that concentration is 20mg/L, isothermal adsorption is carried out at 30 DEG C.Fig. 2 a is methylene blue solution
(original), the uv absorption spectra of CFs-1, CFs-2, CFs-3, CFs-4 and CFs-5, Fig. 2 b are CFs-1, CFs-
2, the adsorbance curve graph of CFs-3, CFs-4 and CFs-5 to methylene blue.As a result as it can be seen that adsorbing carbon fiber pair after 72h in
The adsorbance of methylene blue increases to 461.05mg/g by unmodified preceding 168.85mg/g, shows to add two isocyanide of isophorone
Sample after acid esters has better absorption property.
Gained carbon fiber carries out measuring mechanical property, is tested using monoaxial stretching method.Test result such as Fig. 3, warp
The tensile strength of carbon fibers for crossing modified preparation is increased to 49MPa (Fig. 3 a) by 24MPa, and Young's modulus is by unmodified 1.4GPa
Increase to the 3.0GPa (Fig. 3 b) after being modified.
Embodiment 2
It is prepared as follows ethyl alcohol lignin/cellulose acetate base electrostatic spinning carbon fiber:
(1) corn stover is digested into residue ethyl alcohol lignin and cellulose acetate according to mass ratio 40:60 (w/w), be dissolved in
The in the mixed solvent of acetone/n,N-Dimethylformamide (v/v:2:1), after being completely dissolved be added isophorone diisocyanate and
Dibutyl tin dilaurate, the final concentration of 10wt% of isophorone diisocyanate, di lauric dibutyl in reaction solution
The final concentration of 15wt% of the final concentration of 1wt% of tin, ethyl alcohol lignin and cellulose acetate, reacts 72h at 60 DEG C, obtains wooden
Quality/cellulose acetate base spinning solution；
(2) spinning solution that step (1) obtains is prepared into lignin/cellulose acetate base carbon fibre by electrospinning process
Precursor, the condition of electrostatic spinning are as follows: electrostatic pressure 25KV, receiving distance is 25cm, receives rod revolving speed 600r/min, spinning is molten
The fltting speed of liquid is 0.5mL/h；
(3) carbon fiber precursor obtained is placed in tube furnace, is pre-oxidized and be carbonized, in air atmosphere with
The heating rate of 0.2 DEG C/min is warming up to 250 DEG C, and keeps the temperature 720min and carry out pre-oxidation treatment；Then under nitrogen protection with 5
DEG C/rate of min is warming up to 800 DEG C, and keeps the temperature 120min and carry out heating carbonization treatment, obtain lignin/cellulose acetate base
Electrostatic spinning carbon fiber.
Embodiment 3
It is prepared as follows ethyl alcohol lignin/cellulose acetate base electrostatic spinning carbon fiber:
(1) corn stover is digested into residue ethyl alcohol lignin and cellulose acetate according to mass ratio 40:40 (w/w), be dissolved in
The in the mixed solvent of acetone/n,N-Dimethylformamide (v/v:2:1), after being completely dissolved be added isophorone diisocyanate and
Dibutyl tin dilaurate, the final concentration of 12wt% of isophorone diisocyanate, di lauric dibutyl in reaction solution
The final concentration of 25wt% of the final concentration of 2wt% of tin, ethyl alcohol lignin and cellulose acetate, reacts 72h at 60 DEG C, obtains wooden
Quality/cellulose acetate base spinning solution；
(2) spinning solution that step (1) obtains is prepared into lignin/cellulose acetate base carbon fibre by electrospinning process
Precursor, the condition of electrostatic spinning are as follows: electrostatic pressure 20KV, receiving distance is 30cm, receives rod revolving speed 700r/min, spinning is molten
The fltting speed of liquid is 0.8mL/h；
(3) carbon fiber precursor obtained is placed in tube furnace, is pre-oxidized and be carbonized, in air atmosphere with
The heating rate of 0.5 DEG C/min is warming up to 220 DEG C, and keeps the temperature 720min and carry out pre-oxidation treatment；Then under nitrogen protection with 8
DEG C/rate of min is warming up to 1000 DEG C, and keeps the temperature 120min and carry out heating carbonization treatment, obtain lignin/cellulose acetate base
Electrostatic spinning carbon fiber.
Gained carbon fiber electron microscope still maintains excellent form, and methylene blue adsorption number effect is better than being not added with different Fo Er
The lignin of ketone diisocyanate/cellulose acetate base electrostatic spinning carbon fiber.
The preferred embodiment of the present invention has been described in detail above, but the invention be not limited to it is described
Embodiment, those skilled in the art can also make various equivalent on the premise of not violating the inventive spirit of the present invention
Variation or replacement, these equivalent variation or replacement are all included in the scope defined by the claims of the present application.
Claims (10)
1. a kind of lignin/cellulose acetate base electrostatic spinning carbon fiber preparation method will be wooden by electrospinning process
Carbon fiber precursor is made in element/cellulose acetate base spinning solution, then carbon fiber is made through pre-oxidation treatment and carbonization treatment, special
Sign is, by lignin and cellulose acetate in the presence of catalyst and difunctional isocyanates, it is anti-to carry out chemical modification
Lignin/cellulose acetate base the spinning solution should be made.
2. preparation method according to claim 1, which is characterized in that the difunctional isocyanates is isophorone
Diisocyanate, MDI diisocyanate, 1,4- cyclohexane diisocyanate, TDI toluene di-isocyanate(TDI), 1,5- how two isocyanides
Acid esters, methylene diisocyanate, methyl -2,4- diisocyanate, dimer acid diisocyanate, diphenylmethane diisocyanate
One or more of ester, xylylene diisocyanate.
3. preparation method according to claim 1, which is characterized in that the catalyst be dibutyl tin dilaurate,
One of Dibutyltin oxide, stannous octoate.
4. preparation method according to claim 1, which is characterized in that the reaction temperature of the chemical modification reaction is 60
~100 DEG C, the reaction time is 1~10h.
5. preparation method according to claim 1, which is characterized in that in the chemical modification reaction, the wood
Quality and the additional amount of cellulose acetate are 30:70~70:30 in mass ratio, the addition of the lignin and cellulose acetate
Amount is the 10~30% of reaction solution quality.
6. preparation method according to claim 1, which is characterized in that in the chemical modification reaction, described is double
The additional amount of functional group's isocyanates is the 2~20% of reaction solution quality, and the additional amount of the catalyst is reaction solution quality
0.1~5%.
7. preparation method according to claim 1, which is characterized in that in the chemical modification reaction, by lignin
The in the mixed solvent of solvent A and solvent B is dissolved in cellulose acetate, wherein the mixed proportion of solvent A and solvent B are by volume
1~2:1, the mixed solution solvent A/solvent B be acetone/n,N dimethylformamide, glacial acetic acid/n,N dimethylformamide,
Acetone/N, N dimethyl acetamide or glacial acetic acid/N, one of N dimethyl acetamide.
8. preparation method according to claim 1, which is characterized in that in the electrospinning process, electrostatic potential 15
~35KV, receiving distance is 10~35cm, and receiving rod revolving speed is 200~700r/min, and it is 0.1~1mL/h that spinning solution, which pushes away speed,.
9. preparation method according to claim 1, which is characterized in that the pre-oxidation treatment is by carbon fiber precursor
It is pre-oxidized in air atmosphere, pre-oxidation is by room temperature, is warming up to 200~300 DEG C with the rate of 0.01~2.00 DEG C/min,
And 2~10h is kept the temperature at this temperature；The carbonization treatment is will be through pre-oxidized fibers that pre-oxidation treatment obtains in indifferent gas
Body protection is lower to heat carbonization treatment, is warming up to 600~1400 DEG C with 2~10 DEG C/min rate, and at this temperature heat preservation 2~
10h。
10. the lignin that described in any item methods of claim 1~9 are prepared/cellulose acetate base electrostatic spinning carbon
Fiber is preparing the application in adsorbent.
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| CN112195536A (en) * | 2020-09-10 | 2021-01-08 | 扬州市职业大学(扬州市广播电视大学) | Preparation method of full-biomass-based carbon nanofiber |
| CN115595691A (en) * | 2022-11-08 | 2023-01-13 | 哈尔滨体育学院（Cn） | Lignocellulose-based carbon fiber with excellent electrochemical performance and preparation method and application thereof |
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| CN115595691A (en) * | 2022-11-08 | 2023-01-13 | 哈尔滨体育学院（Cn） | Lignocellulose-based carbon fiber with excellent electrochemical performance and preparation method and application thereof |
| CN115595691B (en) * | 2022-11-08 | 2024-04-19 | 哈尔滨体育学院 | Lignocellulose-based carbon fiber with excellent electrochemical performance, and preparation method and application thereof |
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