CN108866669A - A kind of preparation method of modified carbon nano-tube/conducting polypropylene nitrile fiber - Google Patents
A kind of preparation method of modified carbon nano-tube/conducting polypropylene nitrile fiber Download PDFInfo
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- CN108866669A CN108866669A CN201810819296.8A CN201810819296A CN108866669A CN 108866669 A CN108866669 A CN 108866669A CN 201810819296 A CN201810819296 A CN 201810819296A CN 108866669 A CN108866669 A CN 108866669A
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- carbon nano
- modified carbon
- tube
- polypropylene nitrile
- nitrile fiber
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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
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/54—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated nitriles
-
- 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
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Carbon And Carbon Compounds (AREA)
- Inorganic Fibers (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention proposes a kind of modified carbon nano-tube/conducting polypropylene nitrile fiber preparation methods, and steps are as follows：（1）Sour modified carbon nano-tube is dissolved in the hexane solution of t etram-ethyltetravinylcyclotetrasiloxane, is blown into nitrogen, using being placed in after ultrasonic treatment60It is irradiated in the gamma-rays of Co radioactive source, drying is washed after irradiation, obtains graft copolymerization crude product；（2）Step（1）Obtained graft copolymerization crude product is heated to reflux to constant weight using acetone as solvent, obtains grafting carbon nanotube after insoluble matter drying；（3）By step（2）Obtained grafting carbon nanotube, PAN and DMF is mixed and made into spinning solution, and spinning solution progress spinning is obtained modified carbon nano-tube/conducting polypropylene nitrile fiber.Under the catalysis of hydrochloric acid, the amorphous carbon on original carbon nanotubes surface can be oxidized by nitric acid, and generated carbon dioxide and removed.After when surface, amorphous carbon layer is dispelled, the outer surface of carbon nanotube continues to be oxidized by nitric acid, and generates hydroxyl and carboxyl.
Description
Technical field
The present invention relates to fiber preparation fields, and in particular to a kind of system of modified carbon nano-tube/conducting polypropylene nitrile fiber
Preparation Method.
Background technique
Carbon nanotube has high intensity, and calculated value is 100 times of steel, at the same carbon nanotube have it is high tough
Property, it is sufficiently flexible, it is considered to be following super fiber, and meanwhile it is also conductive, the present invention utilizes the performance of carbon nanotube
Prepare modified carbon nano-tube conducting polypropylene nitrile fiber.The growth characteristic of carbon nanotube is that more root balls gather and intertwine with each other, in addition
Carbon nano tube surface feature is similar with graphite, and all insoluble in most solvents, wet performance is poor, if with untreated
Carbon nanotube is added in polymer, then will appear and the problems such as matrix associativity is poor, bad dispersibility.Therefore, how to make nanometer
Carbon pipe is evenly dispersed in the matrix of composite material, and combining closely with matrix is to prepare carbon nanotubes enhancing composite material head
First consider the problems of.
Since the steric hindrance of polymer molecular chain prevents the carboxyl of carbon nano tube surface from effectively reacting, thus it is grafted
Rate is very low, therefore this patent is reached using the method for effective modified carbon nano-tube and is satisfied with grafting rate.
Summary of the invention
The invention proposes a kind of modified carbon nano-tube/conducting polypropylene nitrile fiber preparation methods, solve existing carbon
Nanometer hangs the low problem of grafting rate.
Realize the technical scheme is that：A kind of preparation method of modified carbon nano-tube/conducting polypropylene nitrile fiber, step
It is rapid as follows：
（1）Sour modified carbon nano-tube is dissolved in the hexane solution of t etram-ethyltetravinylcyclotetrasiloxane, nitrogen is blown into
15min, using being placed in after ultrasonic treatment60It is irradiated in the gamma-rays of Co radioactive source, drying is washed after irradiation, obtain grafting altogether
Poly- crude product；
（2）Step（1）Obtained graft copolymerization crude product is heated to reflux to constant weight, obtains after insoluble matter drying using acetone as solvent
To grafting carbon nanotube；
（3）By step（2）Obtained grafting carbon nanotube, PAN（Polyacrylonitrile）It is mixed and made into spinning solution with DMF, by spinning solution
It carries out spinning and obtains modified carbon nano-tube/conducting polypropylene nitrile fiber.
The step（1）The concentration of the hexane solution of middle t etram-ethyltetravinylcyclotetrasiloxane is 0.005-0.01
g/ml。
The step（1）The condition of middle ultrasonic treatment is 20 DEG C of temperature, power 125W, time 12-20h.
The step（1）The condition of middle gamma-ray irradiation is：Radiance 1KGy/h, irradiation time 30-36h.
The step（2）Middle reflux temperature is 50-55 DEG C, and drying temperature is 90-100 DEG C.
The step（1）It is middle acid modified carbon nano-tube preparation method be：Carbon nanotube is placed in the nitric acid of 3 mol/L
60 DEG C of return stirrings for 24 hours, are cooled to room temperature centrifugation gained precipitating and are dissolved in 120 DEG C, handle 6h in 5 mol/L hydrochloric acid, be cooled to room
It is 7 that temperature centrifugation gained precipitating, which is rinsed with deionized water to pH, then be placed on three times with acetone rinsing 60 DEG C, the vacuum of 10mbar it is dry
To constant weight in dry case.
The step（3）The mass ratio of middle grafting carbon nanotube and PAN is（10-15）：（85-90）.
The step（3）Middle spinning process is：Spinning solution is squeezed out under nitrogen 0.3MPa pressure, is reached by metering pump
Spinning nozzle, then enter in sodium thiocyanate water solution coagulating bath through spinning nozzle and solidified, enter in boiling water bath after solidification and is washed
It washs, is then dried by high temperature drying cylinder, package obtains modified carbon nano-tube/conducting polypropylene nitrile fiber.
It is as follows that carbon nanotube is acidified principle：
。
The beneficial effects of the invention are as follows：Carbon nanotube in nitration mixture purification process, is played the main of oxidation by the present invention
It is nitric acid, the effect of hydrochloric acid is to be catalyzed the oxidation reaction and dissolved metal ions of nitric acid.Catalyst n i/Mo/MgO is first by nitric acid
Then oxidation reacts with hydrochloric acid and generates NiCl2、MgCl2(MoO2)Cl2, these compounds can be dissolved in nitration mixture, can by filtering
To remove.Under the catalysis of hydrochloric acid, the amorphous carbon on original carbon nanotubes surface can be oxidized by nitric acid, generate carbon dioxide and
It removes.After when surface, amorphous carbon layer is dispelled, the outer surface of carbon nanotube continues to be oxidized by nitric acid, and generates hydroxyl and carboxyl.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is that carbon nanotube is acidified schematic diagram.
Fig. 2 is infrared spectrogram after the acidification of 1 carbon nanotube of embodiment.
Fig. 3 is that 1 carbon nanotube of embodiment is acidified the graceful spectrogram of post-tensioning.
Fig. 4 is carbon nanotube radiation grafting schematic diagram.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Those of ordinary skill in the art's every other embodiment obtained under that premise of not paying creative labor, belongs to this hair
The range of bright protection.
Embodiment 1
A kind of preparation method of modified carbon nano-tube/conducting polypropylene nitrile fiber, steps are as follows：
It weighs 60 DEG C of return stirrings of nitric acid that a certain amount of carbon nanotube is dissolved in 3 mol/L for 24 hours, it is heavy to be cooled to room temperature centrifugation gained
Shallow lake is dissolved in 120 DEG C, 6h in 5 mol/L hydrochloric acid, and being cooled to room temperature centrifugation gained precipitating and being rinsed with deionized water to PH is 7, then is used
Acetone rinsing is placed on 60 DEG C three times（10mbar）To constant weight in vacuum oven, weigh constant weight carbon nanotubes be placed in it is transparent
In ampere bottle, then pour into 100ml（0.005g/ml）T etram-ethyltetravinylcyclotetrasiloxane hexane solution, be blown into nitrogen
15min is placed on excluding dissolved oxygen through 20 DEG C, 125W ultrasound60In the gamma-rays of Co radioactive source, radiance 1KGy/h, warp
After 30h irradiation, irradiated reaction mass is taken out, repeatedly rinses to be placed in baking oven with deionized water water and dries to constant weight, i.e.,
Obtain graft copolymerization crude product.A certain amount of graft copolymerization crude product is weighed, is placed in Soxhlet extractor, using acetone as solvent, is added
Heat is back to constant weight (remove tetramethyl tetravinyl silane), reflux temperature be 50 DEG C, drying temperature be 90 DEG C, by it is remaining not
Molten object dries to constant weight to get graft copolymer.
Weight W when sample drying before radiation treatment1, weight W after sample drying after radiation washing extraction2, carry out grafting rate calculating and connect
Branch rate (%)=(W2-W1)/W1× 100% dose of radiation and grafting rate relational graph as seen from the figure.
Modified carbon nano-tube conducting polypropylene nitrile fiber is prepared using wet process, by the modified carbon nano-tube conductive powder body of preparation
It is mixed respectively in proportion with PAN, the mass ratio of grafting carbon nanotube and PAN are 10：90, appropriate DMF is added（N, N- diformazan
Base amide）It is packed into serum storage tank, leads to certain pressure after compressing collet stirring（0.3MPa）Nitrogen by spinning solution squeeze out by meter
Amount pump reaches spinning nozzle, then enters in sodium thiocyanate water solution (25% solubility) coagulating bath through spinning nozzle, in coagulating bath through appropriate
Solidification, enter boiling water bath by roller, the rate of control front and back two makes fiber obtain certain drawing-off simultaneously also to fiber progress
Certain washing.Then roller enters lower washing together carries out the DMF solvent wash clean of fibrous inside by high temperature drying cylinder
It is dry, most package.
Use the modified carbon nano-tube conducting polypropylene nitrile fabric resistor rate of this method preparation for 5.86 × 108Ω cm,
Average fracture strength 5.88cN/tex, average extension at break 7.21%.
Embodiment 2
A kind of preparation method of modified carbon nano-tube/conducting polypropylene nitrile fiber, steps are as follows：
It weighs 60 DEG C of return stirrings of nitric acid that a certain amount of carbon nanotube is dissolved in 3 mol/L for 24 hours, it is heavy to be cooled to room temperature centrifugation gained
Shallow lake is dissolved in 6h in 120 DEG C of 5 mol/L hydrochloric acid, and being cooled to room temperature centrifugation gained precipitating and being rinsed with deionized water to PH is 7, then with third
Ketone, which flushes three times, is placed on 60 DEG C（10mbar）To constant weight in vacuum oven, weighs constant weight carbon nanotubes and be placed in transparent peace
It trains in bottle, then pours into 100ml（0.008g/ml）T etram-ethyltetravinylcyclotetrasiloxane hexane solution, be blown into nitrogen
15min is placed on excluding dissolved oxygen through 20 DEG C, 125W ultrasound60In the gamma-rays of Co radioactive source, radiance 1KGy/h, warp
After 32h irradiation, irradiated reaction mass is taken out, repeatedly rinses to be placed in baking oven with deionized water water and dries to constant weight, i.e.,
Obtain graft copolymerization crude product.A certain amount of graft copolymerization crude product is weighed, is placed in Soxhlet extractor, using acetone as solvent, is added
Heat is back to constant weight (remove tetramethyl tetravinyl silane), reflux temperature be 53 DEG C, drying temperature be 95 DEG C, by it is remaining not
Molten object dries to constant weight to get graft copolymer.
Weight W when sample drying before radiation treatment1, weight W after sample drying after radiation washing extraction2, carry out grafting rate calculating and connect
Branch rate (%)=(W2-W1)/W1× 100% dose of radiation and grafting rate relational graph as seen from the figure.
Modified carbon nano-tube conducting polypropylene nitrile fiber is prepared using wet process, by the modified carbon nano-tube conductive powder body of preparation
It is mixed respectively in proportion with PAN, the mass ratio of grafting carbon nanotube and PAN are 12：88, appropriate DMF is added（N, N- diformazan
Base amide）It is packed into serum storage tank, leads to certain pressure after compressing collet stirring（0.3MPa）Nitrogen by spinning solution squeeze out by meter
Amount pump reaches spinning nozzle, then enters in sodium thiocyanate water solution (28% solubility) coagulating bath through spinning nozzle, in coagulating bath through appropriate
Solidification, enter boiling water bath by roller, the rate of control front and back two makes fiber obtain certain drawing-off simultaneously also to fiber progress
Certain washing.Then roller enters lower washing together carries out the DMF solvent wash clean of fibrous inside by high temperature drying cylinder
It is dry, most package.
Embodiment 3
A kind of preparation method of modified carbon nano-tube/conducting polypropylene nitrile fiber, steps are as follows：
It weighs 60 DEG C of return stirrings of nitric acid that a certain amount of carbon nanotube is dissolved in 3 mol/L for 24 hours, it is heavy to be cooled to room temperature centrifugation gained
Shallow lake is dissolved in 120 DEG C, 6h in 5 mol/L hydrochloric acid, and being cooled to room temperature centrifugation gained precipitating and being rinsed with deionized water to PH is 7, then is used
Acetone rinsing is placed on 60 DEG C three times（10mbar）To constant weight in vacuum oven, weigh constant weight carbon nanotubes be placed in it is transparent
In ampere bottle, then pour into 100ml（0.01g/ml）T etram-ethyltetravinylcyclotetrasiloxane hexane solution, be blown into nitrogen
15min is placed on excluding dissolved oxygen through 20 DEG C, 125W ultrasound60In the gamma-rays of Co radioactive source, radiance 1KGy/h, warp
After 6h irradiation, irradiated reaction mass is taken out, repeatedly rinsed with deionized water water be placed in baking oven dry to constant weight to get
Graft copolymerization crude product.A certain amount of graft copolymerization crude product is weighed, is placed in Soxhlet extractor, using acetone as solvent, heating
Be back to constant weight (remove tetramethyl tetravinyl silane), reflux temperature be 55 DEG C, drying temperature be 100 DEG C, by it is remaining not
Molten object dries to constant weight to get graft copolymer.
Weight W when sample drying before radiation treatment1, weight W after sample drying after radiation washing extraction2, carry out grafting rate calculating and connect
Branch rate (%)=(W2-W1)/W1× 100% dose of radiation and grafting rate relational graph as seen from the figure.
Modified carbon nano-tube conducting polypropylene nitrile fiber is prepared using wet process, by the modified carbon nano-tube conductive powder body of preparation
It is mixed respectively in proportion with PAN, the mass ratio of grafting carbon nanotube and PAN are 15：85, appropriate DMF is added（N, N- diformazan
Base amide）It is packed into serum storage tank, leads to certain pressure after compressing collet stirring（0.3MPa）Nitrogen by spinning solution squeeze out by meter
Amount pump reaches spinning nozzle, then enters in sodium thiocyanate water solution (30% solubility) coagulating bath through spinning nozzle, in coagulating bath through appropriate
Solidification, enter boiling water bath by roller, the rate of control front and back two makes fiber obtain certain drawing-off simultaneously also to fiber progress
Certain washing.Then roller enters lower washing together carries out the DMF solvent wash clean of fibrous inside by high temperature drying cylinder
It is dry, most package.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of modified carbon nano-tube/conducting polypropylene nitrile fiber preparation method, it is characterised in that steps are as follows：
（1）Sour modified carbon nano-tube is dissolved in the hexane solution of t etram-ethyltetravinylcyclotetrasiloxane, nitrogen is blown into
15min, using being placed in after ultrasonic treatment60It is irradiated in the gamma-rays of Co radioactive source, drying is washed after irradiation, obtain grafting altogether
Poly- crude product；
（2）Step（1）Obtained graft copolymerization crude product is heated to reflux to constant weight, obtains after insoluble matter drying using acetone as solvent
To grafting carbon nanotube；
（3）By step（2）Obtained grafting carbon nanotube, PAN and DMF is mixed and made into spinning solution, and spinning solution progress spinning is obtained
To modified carbon nano-tube/conducting polypropylene nitrile fiber.
2. modified carbon nano-tube according to claim 1/conducting polypropylene nitrile fiber preparation method, which is characterized in that
The step（1）The concentration of the hexane solution of middle t etram-ethyltetravinylcyclotetrasiloxane is 0.005-0.01 g/ml.
3. modified carbon nano-tube according to claim 1/conducting polypropylene nitrile fiber preparation method, it is characterised in that：
The step（1）The condition of middle ultrasonic treatment is that temperature is 20 DEG C, power 125W, time 12-20h.
4. modified carbon nano-tube according to claim 1/conducting polypropylene nitrile fiber preparation method, which is characterized in that
The step（1）The condition of middle gamma-ray irradiation is：Radiance 1KGy/h, irradiation time 30-36h.
5. modified carbon nano-tube according to claim 1/conducting polypropylene nitrile fiber preparation method, it is characterised in that：
The step（2）Middle reflux temperature is 50-55 DEG C, and drying temperature is 90-100 DEG C.
6. modified carbon nano-tube according to claim 1-5/conducting polypropylene nitrile fiber preparation method, special
Sign is, the step（1）It is middle acid modified carbon nano-tube preparation method be：Carbon nanotube is placed in the nitric acid of 3 mol/L
60 DEG C of return stirrings for 24 hours, are cooled to room temperature centrifugation gained precipitating and are dissolved in 120 DEG C, handle 6h in 5 mol/L hydrochloric acid, be cooled to room
It is 7 that temperature centrifugation gained precipitating, which is rinsed with deionized water to pH, then be placed on three times with acetone rinsing 60 DEG C, the vacuum of 10mbar it is dry
To constant weight in dry case.
7. modified carbon nano-tube according to claim 1-5/conducting polypropylene nitrile fiber preparation method, special
Sign is, the step（3）The mass ratio of middle grafting carbon nanotube and PAN is（10-15）：（85-90）.
8. modified carbon nano-tube according to claim 1-5/conducting polypropylene nitrile fiber preparation method, special
Sign is, the step（3）Middle spinning process is：Spinning solution is squeezed out under nitrogen 0.3MPa pressure, is reached by metering pump
Spinning nozzle, then enter in sodium thiocyanate water solution coagulating bath through spinning nozzle and solidified, enter in boiling water bath after solidification and is washed
It washs, is then dried by high temperature drying cylinder, package obtains modified carbon nano-tube/conducting polypropylene nitrile fiber.
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| CN109518306A (en) * | 2018-12-12 | 2019-03-26 | 深圳烯湾科技有限公司 | Modified carbon nano tube fiber and its preparation method and application |
| CN112864435A (en) * | 2021-01-08 | 2021-05-28 | 杭州廖仕科技有限公司 | Preparation method and application of composite fiber membrane of carbon nanotube grafted polyacrylonitrile fiber |
| CN112981582A (en) * | 2021-02-09 | 2021-06-18 | 华中科技大学 | Temperature control fiber integrating heat superconducting and refrigerating functions and preparation method and application thereof |
| CN114427125A (en) * | 2020-10-29 | 2022-05-03 | 中国石油化工股份有限公司 | Carbon nano tube antistatic acrylic fiber and preparation method thereof |
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| CN114427125A (en) * | 2020-10-29 | 2022-05-03 | 中国石油化工股份有限公司 | Carbon nano tube antistatic acrylic fiber and preparation method thereof |
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| CN108866669B (en) | 2020-09-04 |
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