CN116121903A - Method for assisting carbon nano tube dispersion wet spinning fiber formation by double polymers - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 72
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 72
- 239000000835 fiber Substances 0.000 title claims abstract description 60
- 229920000642 polymer Polymers 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000002166 wet spinning Methods 0.000 title claims abstract description 12
- 230000015572 biosynthetic process Effects 0.000 title description 8
- 239000006185 dispersion Substances 0.000 title description 8
- 239000000243 solution Substances 0.000 claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 229920003235 aromatic polyamide Polymers 0.000 claims abstract description 11
- 238000009987 spinning Methods 0.000 claims abstract description 11
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 7
- 229920006231 aramid fiber Polymers 0.000 claims abstract description 5
- 230000003647 oxidation Effects 0.000 claims abstract description 3
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 3
- 230000001112 coagulating effect Effects 0.000 claims description 11
- 230000015271 coagulation Effects 0.000 claims description 9
- 238000005345 coagulation Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000002048 multi walled nanotube Substances 0.000 claims description 2
- 239000002109 single walled nanotube Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 7
- 239000011550 stock solution Substances 0.000 abstract description 6
- 239000004744 fabric Substances 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
- 238000003760 magnetic stirring Methods 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 229910017604 nitric acid Inorganic materials 0.000 description 5
- 230000001590 oxidative effect Effects 0.000 description 5
- 238000000967 suction filtration Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 229920000271 Kevlar® Polymers 0.000 description 3
- 230000003993 interaction Effects 0.000 description 3
- 239000004761 kevlar Substances 0.000 description 3
- 108010005939 Ciliary Neurotrophic Factor Proteins 0.000 description 2
- 102100031614 Ciliary neurotrophic factor Human genes 0.000 description 2
- 239000004760 aramid Substances 0.000 description 2
- 230000001419 dependent effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007847 structural defect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
- D01F6/905—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides of aromatic polyamides
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Artificial Filaments (AREA)
Abstract
A method for dispersing and wet spinning carbon nano tubes into fibers by using a double polymer, which comprises the following steps: uniformly dispersing the modified carbon nano tube subjected to purification and oxidation treatment at 300-400 ℃ in a concentrated sulfuric acid solution of para-aramid fiber or meta-aramid fiber to form spinning stock solution; the spinning dope is then injected into the polyvinyl alcohol deionized water solution at a uniform speed through an injector, and after the replacement is completed, the fibers are dried and collected. The invention realizes the fiber forming preparation of the industrial carbon nano tube on the basis of ensuring the fiber performance of the carbon nano tube, has universality and universality, can realize the large-scale preparation of the carbon nano tube fiber, and has wide application scenes in the aspects of special application, special fabrics and the like.
Description
Technical Field
The invention belongs to the field of spinning methods and processes, and particularly relates to a method for forming fibers by dispersing carbon nano tubes with the assistance of a double polymer through wet spinning.
Background
The carbon nanotube fiber is a macroscopic continuous fiber material with a micrometer diameter, which is constructed by taking nano-scale carbon nanotubes as assembly units.
The current preparation method of carbon nanotube fiber mainly comprises carbon nanotube gas phase fiber formation, carbon nanotube array fiber formation and carbon nanotube wet (solution) fiber formation, wherein the carbon nanotube wet (solution) fiber formation technology is the easiest to industrialize, and has achieved a certain result on other polymers.
In order to realize industrialization, industrialization and batch preparation of the synthesis of the carbon nanotube fibers, a wet-process fiber forming technology of the carbon nanotubes is considered.
At present, the performances of the carbon nanotube fiber and the single carbon nanotube are still greatly different, which indicates that the mechanical strength of the carbon nanotube fiber is not mainly dependent on the mechanical strength of the single carbon nanotube, but is dependent on the micro-assembly structure of the carbon nanotube.
Because the specific surface area of the carbon nano tube is large and the interaction force is strong, the carbon nano tube is easy to generate winding agglomeration, so that the carbon nano tube is difficult to disperse and the wide application of the carbon nano tube is limited. The performance of the carbon nano tube fiber is closely related to the interaction force among the carbon nano tubes in the carbon nano tube fiber, the contact area of the carbon nano tubes distributed in disorder is small, the interaction force among the carbon nano tubes is weak, and structural defects are easily formed in the fiber, so that the mechanical property, the electric conductivity and the like are greatly reduced.
In summary, the existing carbon nanotube fiber forming process is difficult to realize industrial production and preparation of carbon nanotube fibers due to factors such as special materials or equipment, and the performances of the obtained fibers are quite different from those of the obtained fibers of the single carbon nanotubes. There is a need for a novel and versatile carbon nanotube assembly fiber formation technique.
Disclosure of Invention
In order to solve the problems, the invention provides a method for assisting carbon nano tube dispersion wet spinning to form fiber by using a double polymer and application thereof.
The invention is realized by the following technical scheme.
The invention relates to a method for preparing fiber by dispersing and wet spinning carbon nano tubes with the assistance of a double polymer, which comprises the following steps.
(1) The polymer a was placed in concentrated sulfuric acid and left to dissolve completely, giving solution a.
(2) And (3) placing the carbon nano tube in a muffle furnace, purifying at 300-400 ℃, and performing oxidation treatment to functionalize the carbon nano tube to obtain the modified carbon nano tube.
(3) Uniformly dispersing the modified carbon nanotubes in the step (2) in the solution A in the step (1) to obtain a solution B serving as a spinning solution.
(4) Polymer B was fully dissolved in deionized water at a weight percentage of 0.99% -10.7% to serve as a coagulation bath.
(5) Solution B, the spin dope, is injected into the coagulation bath through the injector at a uniform rate and then waits for its displacement in the coagulation bath to dry and collect the fibers.
The solution B (spinning solution) prepared in the steps (1) - (3) comprises, by weight, 0.05% -0.22% of polymer A, 95.9% -99.4% of concentrated sulfuric acid and 0.5% -3.8% of modified carbon nanotubes.
The polymer A comprises one or two combinations of para-aramid fiber or meta-aramid fiber; the polymer B is polyvinyl alcohol; the concentrated sulfuric acid is 95% -98% of aqueous solution; the modified carbon nanotube is an oxidized carbon nanotube, and the carbon nanotube comprises one or more combinations of single-wall carbon nanotubes or multi-wall carbon nanotubes.
The invention realizes the fiber forming preparation of the industrial carbon nano tube on the basis of ensuring the fiber performance of the carbon nano tube, has universality and universality, can realize the large-scale preparation of the carbon nano tube fiber, and has wide application scenes in the aspects of special application, special fabrics and the like.
Drawings
FIG. 1 is a graph showing the overall topography of the sample surface according to examples 2-5 of the present invention. Wherein, P1-CNTF, P2-CNTF, P3-CNTF, and P4-CNTF correspond to examples 2, 3, 4, and 5.
FIG. 2 is an enlarged partial topography of the sample surface according to examples 2-5 of the present invention. Wherein, P1-CNTF, P2-CNTF, P3-CNTF, and P4-CNTF correspond to examples 2, 3, 4, and 5.
FIG. 3 is a graph showing the thermal weight loss of the samples according to examples 1 to 5 of the present invention. Wherein CNTF, P1-CNTF, P2-CNTF, P3-CNTF, and P4-CNTF correspond to examples 1, 2, 3, 4, and 5.
FIG. 4 is a graph showing the stress profile of the samples according to examples 2-5 of the present invention. Wherein, P1-CNTF, P2-CNTF, P3-CNTF, and P4-CNTF correspond to examples 2, 3, 4, and 5.
FIG. 5 is a graph showing strain curves of the samples according to examples 2 to 5 of the present invention. Wherein, P1-CNTF, P2-CNTF, P3-CNTF, and P4-CNTF correspond to examples 2, 3, 4, and 5.
FIG. 6 is a graph showing the conductivity of the samples according to examples 2-5 of the present invention. Wherein, P1-CNTF, P2-CNTF, P3-CNTF, and P4-CNTF correspond to examples 2, 3, 4, and 5.
Description of the embodiments
The invention will be further illustrated by the following examples.
Example 1
A method for preparing polymer carbon nano tube fiber by using a double polymer to assist carbon nano tube dispersion wet spinning fiber forming method comprises the following steps.
(1) 1.5g of para-aramid kevlar (para-aramid fiber) was put into 500ml of 98% concentrated sulfuric acid for 5-7 days until completely dissolved to obtain solution A.
(2) Purifying the carbon nano tube in a muffle furnace at 400 ℃ for 2 hours, oxidizing the carbon nano tube in a mixed solution of 98% concentrated sulfuric acid and 70% concentrated nitric acid with a volume ratio of 3:1 for 1 hour, washing the obtained modified carbon nano tube with deionized water for 3 times, and then performing suction filtration and drying to obtain the modified carbon nano tube.
(3) And taking out 20g of the solution A, adding 0.6g of modified carbon nano tubes, and fully dispersing the modified carbon nano tubes in the solution A by magnetic stirring to obtain a solution B, namely the polymer spinning stock solution.
(4) 1L of deionized water was poured into the water tank as a coagulation bath.
(5) The obtained solution B is sucked by a syringe with the diameter of 22.25 and mm and the capacity of 10 mL, is pushed into the coagulating bath at a constant speed by a stepping motor, and is dried and collected after the fiber is replaced in the coagulating bath, so that the polymer carbon nanotube fiber is marked as CNTF.
Example 2
A method for preparing polymer carbon nano tube fiber by using a double polymer to assist carbon nano tube dispersion wet spinning fiber forming method comprises the following steps.
(1) 1.5g of para-aramid kevlar (para-aramid fiber) was put into 500ml of 98% concentrated sulfuric acid for 5-7 days until completely dissolved to obtain solution A.
(2) Purifying the carbon nano tube in a muffle furnace at 400 ℃ for 2 hours, oxidizing the carbon nano tube in a mixed solution of 98% concentrated sulfuric acid and 70% concentrated nitric acid with a volume ratio of 3:1 for 1 hour, washing the obtained modified carbon nano tube with deionized water for 3 times, and then performing suction filtration and drying to obtain the modified carbon nano tube.
(3) And taking out 20g of the solution A, adding 0.6g of modified carbon nano tubes, and fully dispersing the modified carbon nano tubes in the solution A by magnetic stirring to obtain a solution B, namely the polymer spinning stock solution.
(4) And adding 2g of polyvinyl alcohol crystals into 100ml of deionized water, and fully dissolving in a water tank to obtain a solution C, namely the polymer coagulation bath.
(5) The obtained solution B is sucked by a syringe with the diameter of 22.25 and mm and the capacity of 10 mL, is pushed into the solution C at a constant speed by a stepping motor, and is dried and collected after the fiber is replaced in a coagulating bath, so that the double polymer carbon nano tube fiber is obtained and is marked as P1-CNTF.
Example 3
A method for preparing polymer carbon nano tube fiber by using a double polymer to assist carbon nano tube dispersion wet spinning fiber forming method comprises the following steps.
(1) 1.5g of para-aramid kevlar (para-aramid fiber) was put into 500ml of 98% concentrated sulfuric acid for 5-7 days until completely dissolved to obtain solution A.
(2) Purifying the carbon nano tube in a muffle furnace at 400 ℃ for 2 hours, oxidizing the carbon nano tube in a mixed solution of 98% concentrated sulfuric acid and 70% concentrated nitric acid with a volume ratio of 3:1 for 1 hour, washing the obtained modified carbon nano tube with deionized water for 3 times, and then performing suction filtration and drying to obtain the modified carbon nano tube.
(3) And taking out 20g of the solution A, adding 0.6g of modified carbon nano tubes, and fully dispersing the modified carbon nano tubes in the solution A by magnetic stirring to obtain a solution B, namely the polymer spinning stock solution.
(4) Adding 4g of polyvinyl alcohol crystals into 100ml of deionized water, and fully dissolving in a water tank to obtain solution C, namely the polymer coagulation bath.
(5) The obtained solution B is sucked by a syringe with the diameter of 22.25 and mm and the capacity of 10 mL, is pushed into the coagulating bath at a constant speed by a stepping motor, and is dried and collected after the fiber is replaced in the coagulating bath, so that the double polymer carbon nano tube fiber is obtained and is marked as P2-CNTF.
Example 4
A method for preparing polymer carbon nano tube fiber by using a double polymer to assist carbon nano tube dispersion wet spinning fiber forming method comprises the following steps.
(1) 1.5g of aramid 1313 (meta-aramid fiber) was put into 500ml of 98% concentrated sulfuric acid for 5-7 days to be completely dissolved to obtain solution A.
(2) Purifying the carbon nano tube in a muffle furnace at 400 ℃ for 2 hours, oxidizing the carbon nano tube in a mixed solution of 98% concentrated sulfuric acid and 70% concentrated nitric acid with a volume ratio of 3:1 for 1 hour, washing the obtained modified carbon nano tube with deionized water for 3 times, and then performing suction filtration and drying to obtain the modified carbon nano tube.
(3) And taking out 20g of the solution A, adding 0.6g of modified carbon nano tubes, and fully dispersing the modified carbon nano tubes in the solution A by magnetic stirring to obtain a solution B, namely the polymer spinning stock solution.
(4) 6g of polyvinyl alcohol crystal is added into 100ml of deionized water to be fully dissolved in a water tank to obtain solution C, namely the polymer coagulation bath.
(5) The obtained solution B is sucked by a syringe with the diameter of 22.25 and mm and the capacity of 10 mL, is pushed into the coagulating bath at a constant speed by a stepping motor, and is dried and collected after the fiber is replaced in the coagulating bath, so that the double polymer carbon nano tube fiber is obtained and is marked as P3-CNTF.
Example 5
A method for preparing polymer carbon nano tube fiber by using a double polymer to assist carbon nano tube dispersion wet spinning fiber forming method comprises the following steps.
(1) 1.5g of aramid 1313 (meta-aramid fiber) was put into 500ml of 98% concentrated sulfuric acid for 5-7 days to be completely dissolved to obtain solution A.
(2) Purifying the carbon nano tube in a muffle furnace at 400 ℃ for 2 hours, oxidizing the carbon nano tube in a mixed solution of 98% concentrated sulfuric acid and 70% concentrated nitric acid with a volume ratio of 3:1 for 1 hour, washing the obtained modified carbon nano tube with deionized water for 3 times, and then performing suction filtration and drying to obtain the modified carbon nano tube.
(3) And taking out 20g of the solution A, adding 0.6g of modified carbon nano tubes, and fully dispersing the modified carbon nano tubes in the solution A by magnetic stirring to obtain a solution B, namely the polymer spinning stock solution.
(4) And adding 8g of polyvinyl alcohol crystals into 100ml of deionized water, and fully dissolving in a water tank to obtain a solution C, namely the polymer coagulation bath.
(5) The obtained solution B is sucked by a syringe with the diameter of 22.25 and mm and the capacity of 10 mL, is pushed into the coagulating bath at a constant speed by a stepping motor, and is dried and collected after the fiber is replaced in the coagulating bath, so that the double polymer carbon nano tube fiber is obtained and is marked as P4-CNTF.
Claims (1)
1. A method for forming fibers by dispersing and wet spinning carbon nano tubes with assistance of double polymers is characterized by comprising the following steps:
(1) Placing the polymer A in concentrated sulfuric acid, and completely dissolving to obtain a solution A;
(2) Placing the carbon nano tube in a muffle furnace, purifying at 300-400 ℃, and performing oxidation treatment to functionalize the carbon nano tube to obtain a modified carbon nano tube;
(3) Uniformly dispersing the modified carbon nanotubes in the step (2) in the solution A in the step (1) to obtain a solution B serving as spinning solution;
(4) Fully dissolving a polymer B into deionized water according to the weight percentage of 0.99-10.7%, and taking the polymer B as a coagulation bath;
(5) Injecting the solution B into the coagulating bath at a uniform speed through a syringe, and then waiting for the solution B to finish replacement in the coagulating bath, and drying and collecting the fibers;
the solution B prepared in the steps (1) - (3) comprises 0.05% -0.22% of polymer A, 95.9% -99.4% of concentrated sulfuric acid and 0.5% -3.8% of modified carbon nano-tube by weight percent;
the polymer A comprises one or two combinations of para-aramid fiber or meta-aramid fiber; the polymer B is polyvinyl alcohol; the concentrated sulfuric acid is 95% -98% of aqueous solution; the carbon nanotubes include one or more combinations of single-walled carbon nanotubes or multi-walled carbon nanotubes.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020096139A (en) * | 2001-06-18 | 2002-12-31 | 엘지전자 주식회사 | One-directional aligned carbon nanotube micro string and its fabricating method |
| KR20100052767A (en) * | 2008-11-11 | 2010-05-20 | 주식회사 코오롱 | Method of manufacturing composite fiber of carbon nanotube and aramid |
| KR20120129040A (en) * | 2011-05-18 | 2012-11-28 | 충남대학교산학협력단 | Carbon nanotube fibers and method of preparing the same |
| US20140363669A1 (en) * | 2011-09-07 | 2014-12-11 | William Marsh Rice University | Carbon nanotubes fiber having low resistivity, high modulus and/or high thermal conductivity and a method of preparing such fibers by spinning using a fiber spin-dope |
| WO2017191887A1 (en) * | 2016-05-04 | 2017-11-09 | 재단법인차세대융합기술연구원 | Method for producing graphene oxide/carbon nanotube composite fiber, graphene oxide/graphene composite fiber or graphene oxide/graphene/carbon nanotube composite fiber using wet spinning process |
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- 2023-04-10 CN CN202310375028.2A patent/CN116121903A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20020096139A (en) * | 2001-06-18 | 2002-12-31 | 엘지전자 주식회사 | One-directional aligned carbon nanotube micro string and its fabricating method |
| KR20100052767A (en) * | 2008-11-11 | 2010-05-20 | 주식회사 코오롱 | Method of manufacturing composite fiber of carbon nanotube and aramid |
| KR20120129040A (en) * | 2011-05-18 | 2012-11-28 | 충남대학교산학협력단 | Carbon nanotube fibers and method of preparing the same |
| US20140363669A1 (en) * | 2011-09-07 | 2014-12-11 | William Marsh Rice University | Carbon nanotubes fiber having low resistivity, high modulus and/or high thermal conductivity and a method of preparing such fibers by spinning using a fiber spin-dope |
| WO2017191887A1 (en) * | 2016-05-04 | 2017-11-09 | 재단법인차세대융합기술연구원 | Method for producing graphene oxide/carbon nanotube composite fiber, graphene oxide/graphene composite fiber or graphene oxide/graphene/carbon nanotube composite fiber using wet spinning process |
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