CN109943920B - Method for preparing carbon nanofibers by electrostatic blending of polyacrylonitrile/lignin - Google Patents
Method for preparing carbon nanofibers by electrostatic blending of polyacrylonitrile/lignin Download PDFInfo
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Abstract
The invention discloses a method for preparing carbon nanofibers by electrostatic blending of polyacrylonitrile/lignin. According to the method, after the lignin is subjected to acetylation and graft modification, the lignin has good compatibility with polyacrylonitrile, the spinnability of a polyacrylonitrile/lignin mixed solution is improved, the diameter of the prepared polyacrylonitrile/lignin nanofiber is 200-350 nm, the thermodynamic property is also improved, and the polyacrylonitrile/lignin is successfully utilized to prepare the carbon nanofiber with good structural performance after preoxidation and carbonization.
Description
Technical Field
The invention relates to the technical field of carbon nanofiber preparation, in particular to a method for preparing carbon nanofibers by electrostatic blending polyacrylonitrile/lignin.
Background
The carbon fiber has excellent performances of low density, high strength, high modulus, high temperature resistance, corrosion resistance and the like, is widely applied to the fields of aerospace, biomedical treatment, sports equipment, automobile parts and the like, and the preparation and application of the carbon fiber also promote the development of scientific and technological economy. The nano-scale carbon fiber endows the carbon fiber with larger porosity and specific surface area, and the application range of the carbon fiber is wider.
Common processes for preparing carbon nanofibers mainly include a drawing method, a self-assembly method, a vapor deposition method, a template synthesis method, an electrostatic spinning method, and the like. The drawing method has higher requirement on the viscosity of the solution, the yield of the self-assembly method and the gas-phase deposition method is not high, the template synthesis method cannot carry out continuous production, and the electrostatic spinning method has better controllability on the aspects of spinning process parameters, nanofiber size and the like and is more superior to other methods in the aspects of efficiency and yield.
Polyacrylonitrile (PAN) fiber is commonly used as a raw material for preparing carbon fiber through electrostatic spinning, with the increasing demand of carbon fiber, PAN as a petroleum derivative is more and more consumed, and the problem of higher cost is more and more prominent, and the finding of a low-cost material as a raw material for preparing carbon fiber is more and more urgent. The lignin has rich sources and high carbon content, can be used as a bio-based material of a carbon fiber raw material, but has a complex molecular structure and is not easy to spin and form. In order to reasonably utilize lignin, chemical modification of lignin and mixed electrospinning with other high polymer materials with better spinnability are used as effective methods for utilizing lignin.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for preparing carbon nanofibers by electrostatic blending of polyacrylonitrile/lignin.
The technical scheme of the invention is as follows: a method for preparing carbon nanofibers by electrostatic blending of polyacrylonitrile/lignin comprises the following steps:
(1) pretreating lignosulfonate to obtain lignin;
(2) performing acetic anhydride acetylation treatment on the lignin obtained in the step (1), and then performing acrylonitrile graft modification treatment;
(3) mixing the lignin treated in the step (2) with polyacrylonitrile, dissolving the obtained mixture in an organic solvent, and preparing a polyacrylonitrile/lignin mixed solution with a solute mass fraction of 8-16%;
(4) performing electrostatic spinning molding on the polyacrylonitrile/lignin mixed solution prepared in the step (3) to prepare a polyacrylonitrile/lignin nanofiber membrane; during electrostatic spinning forming, the voltage is 10-20 kv, the receiving distance is 12-20 cm, and the flow pushing speed is 0.2-2 ml/h;
(5) and (4) pre-oxidizing the polyacrylonitrile/lignin nanofiber membrane prepared in the step (4) in the air, wherein the pre-oxidation temperature is 200-280 ℃, the pre-oxidation time is 0.5-2 h, and the pre-oxidized polyacrylonitrile/lignin nanofiber membrane is heated to 700-1000 ℃ under the protection of nitrogen and carbonized for 2-8 h.
In the step (1), the pretreatment method of the lignosulfonate comprises the following steps: heating and dissolving lignosulfonate in a NaOH solution, filtering to remove impurities, quickly stirring the solution, dropwise adding concentrated sulfuric acid, adjusting the pH value of the solution to 2-4, and centrifugally drying the solution to obtain lignin.
In the step (2), the acetic anhydride acetylation treatment method of lignin comprises the following steps: dissolving the lignin obtained in the step (1) in dimethyl sulfoxide, adding triethylamine, slowly dropwise adding acetic anhydride and continuously stirring, reacting at normal temperature for 2-8 h, placing the reaction product in diethyl ether for precipitation, filtering, washing the filtered solid with ethanol, and drying in vacuum at 50-80 ℃ to obtain acetylated lignin.
In the step (2), the acrylonitrile graft modification treatment method of lignin comprises the following steps: mixing acrylonitrile, azodiisobutyronitrile and dimethyl sulfoxide, heating to 60-90 ℃, and slowly stirring under the protection of nitrogen for not more than 2 hours to obtain a mixed solution; mixing lignin acetylated by acetic anhydride with the mixed solution, and adding CaCl2And H2O2And stirring and reacting for 14-24 hours under the protection of nitrogen.
In the step (3), the mass ratio of the lignin to the Polyacrylonitrile (PAN) is 5: 5-1: 9.
In the step (3), the organic solvent is dimethylformamide solution, dimethyl sulfoxide solution or a mixed solution of dimethylformamide and dimethyl sulfoxide, and the solute mass fraction of the organic solvent is 8-16%.
In the step (4), the ambient temperature of the electrostatic spinning is 10-30 ℃, and the ambient humidity is 20-70%.
In the step (4), the diameter of the electrostatic spinning needle is 0.1-1 mm.
And (5) in the pre-oxidation process of the step (5), applying tension in the same direction to the polyacrylonitrile/lignin nanofiber membrane.
In the pre-oxidation process of the step (5), the temperature rise rate is 5-20 ℃/min.
Compared with the prior art, the invention has the following beneficial effects:
according to the method for preparing the carbon nanofiber by electrostatic blending of polyacrylonitrile/lignin, lignin is used as one of raw materials for preparing the carbon nanofiber, the lignin is rich in source, safe and nontoxic, and the use cost is reduced.
According to the method for preparing the carbon nanofiber by electrostatic blending of polyacrylonitrile/lignin, the lignin is subjected to acetylation and graft modification in advance, so that the compatibility and spinnability of the lignin and a high polymer material are improved.
According to the method for preparing the carbon nanofiber by electrostatic blending of polyacrylonitrile/lignin, the polyacrylonitrile and the lignin are used for preparing the nanofiber membrane by electrostatic blending, the diameter of the prepared polyacrylonitrile/lignin nanofiber membrane is small and can reach 200-350 nm, and the thermodynamic performance is good; the invention successfully prepares the polyacrylonitrile/lignin carbon nanofiber with better morphological characteristics and carbonization degree.
Drawings
FIG. 1 is an electron microscope topography of polyacrylonitrile/lignin nanofibers prepared by the method of example 1.
Fig. 2 is a raman spectrum of polyacrylonitrile/lignin carbon nanofibers prepared by the method of example 2.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
The embodiment of the invention relates to a method for preparing carbon nanofibers by electrostatic blending of polyacrylonitrile/lignin, as shown in fig. 1, the method specifically comprises the following steps:
(1) dissolving 20g of lignosulfonate in 2000ml of 0.5mol/L NaOH solution, stirring until the lignosulfonate is completely dissolved, filtering impurities, slowly dropwise adding concentrated sulfuric acid into the obtained filtrate, continuously stirring, adjusting the pH value to 3, heating to 85 ℃, stirring for a period of time, cooling, precipitating, centrifuging, repeatedly centrifuging and drying for multiple times, and finally drying and grinding to obtain lignin powder.
(2) Dissolving 2g of lignin powder obtained in the step (1) in 40ml of dimethyl sulfoxide (DMSO), cooling after the dissolution is finished, then adding 2ml of Triethylamine (TEA), slowly adding 20ml of acetic anhydride, continuously stirring, and reacting for 6 hours at normal temperature; precipitating the reaction product in ether, centrifuging, washing with ethanol, and drying at 60 deg.C under vacuum to obtain acetylated lignin; adding 5g of Acrylonitrile (AN) and 10mg of Azobisisobutyronitrile (AIBN) into a three-neck round-bottom flask containing 20ml of dimethyl sulfoxide (DMSO), slowly stirring to dissolve the acrylonitrile and the azobisisobutyronitrile, heating to 70 ℃, and stirring for 2 hours under the protection of nitrogen; 2g of acetylated lignin dissolved in 40ml of dimethyl sulfoxide are poured into a round-bottomed flask, then 2g of CaCl2 and 2ml of 30% H are added2O2The reaction was stirred under nitrogen for 24 h.
(3) And (3) mixing the modified lignin and polyacrylonitrile according to the mass ratio of 3: 7, mixing, dissolving and dispersing in 5ml of Dimethylformamide (DMF) to prepare a 12% polyacrylonitrile/lignin mixed solution as an electrostatic spinning solution; and (3) carrying out electrostatic spinning forming on the prepared electrostatic spinning solution by adopting the process conditions that the electrostatic spinning voltage is 15kv, the electrostatic spinning receiving distance is 18cm and the electrostatic spinning flow pushing speed is 0.5ml/h, so as to prepare the polyacrylonitrile/lignin nanofiber membrane.
(4) And placing the obtained polyacrylonitrile/lignin nanofiber membrane in a muffle furnace, heating to 250 ℃ at a speed of 5 ℃/min in the air atmosphere, preserving heat for 2 hours for pre-oxidation, then placing the pre-oxidized polyacrylonitrile/lignin nanofiber membrane in a vacuum tube furnace, heating to 900 ℃ at a speed of 5 ℃/min under the protection of nitrogen, carbonizing, and preserving heat for 2 hours to obtain the polyacrylonitrile/lignin carbon nanofiber.
Example 2
The embodiment of the invention relates to a method for preparing carbon nanofibers by electrostatic blending of polyacrylonitrile/lignin, which specifically comprises the following steps:
(1) dissolving 20g of lignosulfonate in 2000ml of 0.5mol/L NaOH solution, stirring until the lignosulfonate is completely dissolved, filtering impurities, slowly dropwise adding concentrated sulfuric acid into the obtained filtrate, continuously stirring, adjusting the pH value to 3, heating to 85 ℃, stirring for a period of time, cooling, precipitating, centrifuging, repeatedly centrifuging and drying for multiple times, and finally drying and grinding to obtain lignin powder.
(2) Dissolving 2g of lignin powder obtained in the step (1) in 40ml of dimethyl sulfoxide (DMSO), cooling after the dissolution is finished, then adding 2ml of Triethylamine (TEA), slowly adding 30ml of acetic anhydride, continuously stirring, and reacting for 4 hours at 30 ℃; precipitating the reaction product in ether, centrifuging, washing with ethanol, and drying at 60 deg.C under vacuum to obtain acetylated lignin; adding 5g of Acrylonitrile (AN) and 10mg of Azobisisobutyronitrile (AIBN) into a three-neck round-bottom flask containing 20ml of dimethyl sulfoxide (DMSO), slowly stirring to dissolve the acrylonitrile and the azobisisobutyronitrile, heating to 70 ℃, and stirring for 2 hours under the protection of nitrogen; 2g of acetylated lignin dissolved in 40ml of dimethyl sulfoxide are poured into a round-bottomed flask, then 2g of CaCl2 and 2ml of 30% H are added2O2The reaction was stirred under nitrogen for 24 h.
(3) And (2) mixing the modified lignin and polyacrylonitrile according to the mass ratio of 2: 8, mixing, dissolving and dispersing in 5ml of Dimethylformamide (DMF) to prepare a 12% polyacrylonitrile/lignin mixed solution as an electrostatic spinning solution; and (3) carrying out electrostatic spinning forming on the prepared electrostatic spinning solution by adopting the process conditions that the electrostatic spinning voltage is 12kv, the electrostatic spinning receiving distance is 16cm and the electrostatic spinning flow pushing speed is 1ml/h, so as to prepare the polyacrylonitrile/lignin nanofiber membrane.
(4) And placing the obtained polyacrylonitrile/lignin nanofiber membrane in a muffle furnace, heating to 230 ℃ at the speed of 5 ℃/min in the air atmosphere, preserving heat for 2 hours for pre-oxidation, then placing the pre-oxidized polyacrylonitrile/lignin nanofiber membrane in a vacuum tube furnace, heating to 900 ℃ at the speed of 5 ℃/min under the protection of nitrogen, carbonizing, and preserving heat for 2 hours to obtain the polyacrylonitrile/lignin carbon nanofiber.
As shown in fig. 2, it is a raman spectrum of the polyacrylonitrile/lignin carbon nanofiber prepared in this example; in the figure, 1355cm-1The peak is called D peak, which represents disorder and defect condition in the carbon fiber carbonization process, 1589cm-1The peak position G peak shows the integrity of the carbon fiber structure. R is D/G, the carbonization degree and the structural regularity of the fiber are measured, the R value of the polyacrylonitrile/lignin composite carbon fiber is 0.95, the carbonization degree of the fiber is higher, and 2894cm-1The peak appearing is referred to as a 'G' peak, and this peak appears only in the carbon fiber having a higher degree of carbonization.
Example 3
The embodiment of the invention relates to a method for preparing carbon nanofibers by electrostatic blending of polyacrylonitrile/lignin, which specifically comprises the following steps:
(1) dissolving 20g of lignosulfonate in 2000ml of 0.5mol/L NaOH solution, stirring until the lignosulfonate is completely dissolved, filtering impurities, slowly dropwise adding concentrated sulfuric acid into the obtained filtrate, continuously stirring, adjusting the pH value to 3, heating to 85 ℃, stirring for a period of time, cooling, precipitating, centrifuging, repeatedly centrifuging and drying for multiple times, and finally drying and grinding to obtain lignin powder.
(2) Dissolving 2g of lignin powder obtained in the step (1) in 40ml of dimethyl sulfoxide (DMSO), cooling after the dissolution is finished, then adding 2ml of Triethylamine (TEA), slowly adding 40ml of acetic anhydride, continuously stirring, and reacting for 2 hours at normal temperature; precipitating the reaction product in ether, centrifuging, washing with ethanol, and drying at 60 deg.C under vacuum to obtain acetylated lignin; adding 5g of Acrylonitrile (AN) and 10mg of Azobisisobutyronitrile (AIBN) into a three-neck round-bottom flask containing 20ml of dimethyl sulfoxide (DMSO), slowly stirring to dissolve the acrylonitrile and the azobisisobutyronitrile, heating to 70 ℃, and stirring for 2 hours under the protection of nitrogen; 2g of acetylated lignin dissolved in 40ml of dimethyl sulfoxide are poured into a round-bottomed flask, then 2g of CaCl2 and 2ml of 30% H are added2O2The reaction was stirred under nitrogen for 24 h.
(3) And (3) mixing the modified lignin and polyacrylonitrile according to the mass ratio of 1:9, mixing, dissolving and dispersing in 5ml of Dimethylformamide (DMF) to prepare a 12% polyacrylonitrile/lignin mixed solution as an electrostatic spinning solution; and (3) carrying out electrostatic spinning forming on the prepared electrostatic spinning solution by adopting the process conditions that the electrostatic spinning voltage is 12kv, the electrostatic spinning receiving distance is 16cm and the electrostatic spinning flow pushing speed is 2ml/h, so as to prepare the polyacrylonitrile/lignin nanofiber membrane.
(4) And placing the obtained polyacrylonitrile/lignin nanofiber membrane in a muffle furnace, heating to 280 ℃ at a speed of 5 ℃/min in the air atmosphere, preserving heat for 2 hours for pre-oxidation, then placing the pre-oxidized polyacrylonitrile/lignin nanofiber membrane in a vacuum tube furnace, heating to 900 ℃ at a speed of 5 ℃/min under the protection of nitrogen, carbonizing, and preserving heat for 2 hours to obtain the polyacrylonitrile/lignin carbon nanofiber.
As mentioned above, the present invention can be better realized, and the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the scope of the present invention; all equivalent changes and modifications made according to the present disclosure are intended to be covered by the scope of the claims of the present invention.
Claims (9)
1. A method for preparing carbon nanofibers by electrostatic blending of polyacrylonitrile/lignin is characterized by comprising the following steps:
(1) pretreating lignosulfonate to obtain lignin;
(2) dissolving the lignin obtained in the step (1) in dimethyl sulfoxide, adding triethylamine, slowly dropwise adding acetic anhydride and continuously stirring, reacting at normal temperature for 2-8 h, placing a reaction product in diethyl ether for precipitation, filtering, washing the filtered solid with ethanol, drying at 50-80 ℃ in vacuum to obtain acetylated lignin, and performing acrylonitrile graft modification;
(3) mixing the lignin treated in the step (2) with polyacrylonitrile, dissolving the obtained mixture in an organic solvent, and preparing a polyacrylonitrile/lignin mixed solution with a solute mass fraction of 8-16%;
(4) performing electrostatic spinning molding on the polyacrylonitrile/lignin mixed solution prepared in the step (3) to prepare a polyacrylonitrile/lignin nanofiber membrane; during electrostatic spinning forming, the voltage is 10-20 kv, the receiving distance is 12-20 cm, and the flow pushing speed is 0.2-2 ml/h;
(5) and (4) pre-oxidizing the polyacrylonitrile/lignin nanofiber membrane prepared in the step (4) in the air, wherein the pre-oxidation temperature is 200-280 ℃, the pre-oxidation time is 0.5-2 h, and the pre-oxidized polyacrylonitrile/lignin nanofiber membrane is heated to 700-1000 ℃ under the protection of nitrogen and carbonized for 2-8 h.
2. The method for preparing the carbon nanofiber by electrostatically blending polyacrylonitrile/lignin according to claim 1, wherein in the step (1), the pretreatment method of the lignosulfonate comprises the following steps: heating and dissolving lignosulfonate in a NaOH solution, filtering to remove impurities, quickly stirring the solution, dropwise adding concentrated sulfuric acid, adjusting the pH value of the solution to 2-4, and centrifugally drying the solution to obtain lignin.
3. The method for preparing the carbon nanofiber by electrostatically blending polyacrylonitrile/lignin according to claim 1, wherein in the step (2), the method for performing acrylonitrile graft modification on the lignin comprises the following steps: mixing acrylonitrile, azodiisobutyronitrile and dimethyl sulfoxide, heating to 60-90 ℃, and slowly stirring under the protection of nitrogen for not more than 2 hours to obtain a mixed solution; mixing lignin acetylated by acetic anhydride with the mixed solution, and adding CaCl2And H2O2And stirring and reacting for 14-24 hours under the protection of nitrogen.
4. The method for preparing the carbon nanofiber by electrostatically blending polyacrylonitrile/lignin as claimed in claim 1, wherein in the step (3), the mass ratio of lignin to Polyacrylonitrile (PAN) is 5: 5-1: 9.
5. The method for preparing the carbon nanofiber by electrostatically blending polyacrylonitrile/lignin as claimed in claim 1, wherein in the step (3), the organic solvent is dimethylformamide solution, dimethyl sulfoxide solution or a mixed solution of dimethylformamide/dimethyl sulfoxide, and the solute mass fraction of the organic solvent is 8% -16%.
6. The method for preparing the carbon nanofiber by electrostatically blending polyacrylonitrile/lignin according to claim 1, wherein in the step (4), the ambient temperature of electrostatic spinning is 10-30 ℃, and the ambient humidity is 20-70%.
7. The method for preparing the carbon nanofiber by electrostatically blending polyacrylonitrile/lignin as claimed in claim 1, wherein in the step (4), the diameter of a needle of electrostatic spinning is 0.1-1 mm.
8. The method for preparing the carbon nanofiber by electrostatically blending polyacrylonitrile/lignin as claimed in claim 1, wherein in the step (5), the polyacrylonitrile/lignin nanofiber membrane is tensioned in the same direction in the pre-oxidation process.
9. The method for preparing the carbon nanofiber by electrostatically blending polyacrylonitrile/lignin according to claim 1, wherein in the step (5), the temperature rise rate is 5-20 ℃/min in the pre-oxidation process.
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| CN111235697A (en) * | 2020-02-28 | 2020-06-05 | 西安理工大学 | Preparation method of lignin-based carbon material with high wave-absorbing performance |
| CN112853537A (en) * | 2021-01-08 | 2021-05-28 | 杭州神起科技有限公司 | Flame-retardant lignin grafted polyacrylonitrile composite fiber and preparation method thereof |
| CN113332962A (en) * | 2021-03-31 | 2021-09-03 | 陕西科技大学 | Ag-TiO2Preparation method of/CNF/PTFE composite air purification membrane |
| CN114635199B (en) * | 2022-02-07 | 2023-09-26 | 大连大学 | Preparation method of modified lignin compound |
| 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 |
| CN116375392A (en) * | 2023-04-07 | 2023-07-04 | 广东长鑫环保科技有限公司 | Preparation process of material using nano carbonized plant modification and activation technology |
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