CN109056104A - A kind of preparation method of conducting polypropylene fiber - Google Patents
A kind of preparation method of conducting polypropylene fiber Download PDFInfo
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- CN109056104A CN109056104A CN201811104044.3A CN201811104044A CN109056104A CN 109056104 A CN109056104 A CN 109056104A CN 201811104044 A CN201811104044 A CN 201811104044A CN 109056104 A CN109056104 A CN 109056104A
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- -1 polypropylene Polymers 0.000 title claims abstract description 59
- 239000000835 fiber Substances 0.000 title claims abstract description 52
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 50
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 120
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 44
- 239000002270 dispersing agent Substances 0.000 claims abstract description 34
- 239000007822 coupling agent Substances 0.000 claims abstract description 33
- 229920002292 Nylon 6 Polymers 0.000 claims abstract description 25
- 238000012986 modification Methods 0.000 claims abstract description 25
- 230000004048 modification Effects 0.000 claims abstract description 25
- 150000004985 diamines Chemical class 0.000 claims abstract description 15
- DDFGTVSLZJLQEV-UHFFFAOYSA-N [C](C1CCCCC1)C1CCCCC1 Chemical compound [C](C1CCCCC1)C1CCCCC1 DDFGTVSLZJLQEV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004677 Nylon Substances 0.000 claims abstract description 8
- 229920001778 nylon Polymers 0.000 claims abstract description 8
- 239000011499 joint compound Substances 0.000 claims abstract description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 45
- 239000010439 graphite Substances 0.000 claims description 45
- 239000000440 bentonite Substances 0.000 claims description 30
- 229910000278 bentonite Inorganic materials 0.000 claims description 30
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 30
- 239000006185 dispersion Substances 0.000 claims description 30
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 238000001914 filtration Methods 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 239000003999 initiator Substances 0.000 claims description 13
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 12
- 239000003054 catalyst Substances 0.000 claims description 12
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- 150000001336 alkenes Chemical class 0.000 claims description 7
- 230000003647 oxidation Effects 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical group [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 7
- 235000019394 potassium persulphate Nutrition 0.000 claims description 7
- 239000004575 stone Substances 0.000 claims description 7
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- QOSSAOTZNIDXMA-UHFFFAOYSA-N Dicylcohexylcarbodiimide Chemical compound C1CCCCC1N=C=NC1CCCCC1 QOSSAOTZNIDXMA-UHFFFAOYSA-N 0.000 claims description 3
- 150000004645 aluminates Chemical class 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000004020 conductor Substances 0.000 abstract description 6
- 229920002521 macromolecule Polymers 0.000 abstract description 5
- 238000011161 development Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 235000012216 bentonite Nutrition 0.000 description 28
- 238000001035 drying Methods 0.000 description 13
- 239000012065 filter cake Substances 0.000 description 12
- 239000000047 product Substances 0.000 description 12
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N N-phenyl amine Natural products NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 238000012360 testing method Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- VHDPPDRSCMVFAV-UHFFFAOYSA-N n,n-dimethylhexadecan-1-amine;hydrobromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[NH+](C)C VHDPPDRSCMVFAV-UHFFFAOYSA-N 0.000 description 6
- 238000009987 spinning Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 238000005453 pelletization Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 229920000767 polyaniline Polymers 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010036 direct spinning Methods 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 239000004594 Masterbatch (MB) Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 125000002490 anilino group Chemical group [H]N(*)C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229920001197 polyacetylene Polymers 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
Classifications
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
-
- 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
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/12—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a kind of preparation methods of conducting polypropylene fiber, belong to macromolecule conducting material technical field.According to parts by weight, it successively weighs: 40~50 parts of polypropylene agglomerates, 10~15 parts of modification of nylon, 6,5~8 parts of graphene oxides, 10~12 parts of modified alta-muds, 3~5 parts of coupling agents, 4~6 parts of dispersing agents and 2~4 parts of dicyclohexyl carbon Asia diamines;Polypropylene agglomerate is mixed with modification of nylon 6, and graphene oxide is added, modified alta-mud, coupling agent, dispersing agent and dicyclohexyl carbon Asia diamines after being stirred, squeeze out, spinneret is to get conducting polypropylene fiber.The conducting polypropylene fiber of technical solution of the present invention preparation has the characteristics that excellent mechanical property and electric conductivity, has broad prospects in the development of macromolecule conducting material technology industry.
Description
Technical field
The invention discloses a kind of preparation methods of conducting polypropylene fiber, belong to macromolecule conducting material technical field.
Background technique
Conductive fiber is the functional fiber that electrostatic is eliminated by electronics conduction and corona discharge.Conductive fiber is any
In the case of can all eliminate electrostatic in a very short period of time.In addition, the conductive fabric made of conductive fiber, also has excellent lead
The functions such as electric, thermally conductive, shielding, electromagnetic wave absorption are widely used in electronics, the conductive mesh of power industry, conductive work clothes medical treatment
The electric heating clothes of industry, electric face, the electro-magnetic shielding cover of electric heating bandage aviation, aerospace, precision electronics etc..
High molecular material is typically considered insulator, and biography has been broken in the generation of 1970s polyacetylene conductive material
The idea of system produces the macromolecules conductive materials such as polyaniline, polypyrrole, polythiophene in succession later, leads to high molecular material
Electrical property research is also more and more.There are two types of the main methods that conductive fiber is prepared using conduction high polymer.1. conducting polymer
The direct spinning direct spinning of material: wet spinning is generally used, polyaniline is such as made into concentrated solution in certain solidification
Stretch spinning in bath.Here the preparation of polyaniline is aniline under acid medium, with oxidant, such as Ammonium Persulfate 98.5, oxidation polymerization.
2. post treatment method: post treatment method is mainly chemically reacted on general fibre surface, and electroconductive polymer is made to be adsorbed on fiber
Surface makes the conductive energy of general fibre.The preparation method of this kind of conductive fiber is that first general fibre is situated between in aniline acidity
It is impregnated in matter, in order to permeate aniline toward fibrous inside, can heat or be added the sweller of fiber, and urging for copper ions is added
Agent, the fiber after impregnating are immersed in oxidizing agent solution again, the aniline energy rapid polymerization of fiber surface, and the color of fiber is vertical
Light green color is become by brown, and then becomes blackish green, electric conductivity is also best with blackish green color fibre.If not acid adding in aniline
Property substance, after fiber surface is oxidation-treated, color be brown or bronze-colored, conductive capability is poor, or even without conductive capability.
And traditional conducting polypropylene fiber the problem of can not further being promoted there is also mechanical property and electric conductivity, because
This, the shortcomings that how improving conventional conductive polypropylene fibre, develops the conduction poly- third with good comprehensive performance in the hope of exploring
Alkene fiber is problem to be solved.
Summary of the invention
The present invention solves the technical problem of: for conventional conductive polypropylene fibre mechanical property and electric conductivity without
The shortcomings that method is further promoted provides a kind of preparation method of conducting polypropylene fiber.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of conducting polypropylene fiber, specific preparation step are as follows:
(1) graphene oxide dispersion is mixed with ethylenediamine 10:1~15:1 in mass ratio, after being stirred to react, is filtered, washing,
Dry, grinding obtains modified graphene;
(2) modified graphene being mixed with water 1:100~1:180 in mass ratio, ultrasonic disperse obtains modified graphene dispersion liquid,
Modified graphene dispersion liquid is mixed with organobentonite 10:1~12:1 in mass ratio, under microwave condition, after oscillating reactions,
Filtering, dry, grinding obtains modified alta-mud;
(3) expanded graphite is mixed with caprolactam 2:1~3:1 in mass ratio, and is added 10~15 times of expanded graphite quality
N,N-Dimethylformamide, the initiator of 0.1~0.2 times of expanded graphite quality quality and 0.1~0.2 times of expanded graphite quality
Catalyst after being stirred to react, filters, dry, obtains pretreatment expanded graphite, by expanded graphite and the 1:15 in mass ratio of nylon 6~
1:20 mixing, is granulated, obtains modification of nylon 6;
(4) according to parts by weight, it successively weighs: 40~50 parts of polypropylene agglomerates, 10~15 parts of 6,5~8 parts of modification of nylon oxidations
Graphene, 10~12 parts of modified alta-muds, 3~5 parts of coupling agents, 4~6 parts of dispersing agents and 2~4 parts of dicyclohexyl carbon Asia diamines;
Polypropylene agglomerate is mixed with modification of nylon 6, and graphene oxide is added, modified alta-mud, coupling agent, dispersing agent and two hexamethylenes
Base carbon Asia diamines after being stirred, squeezes out, spinneret is to get conducting polypropylene fiber.
Step (1) graphene oxide dispersion is to mix graphene oxide and water 1:100~1:200 in mass ratio
It closes, ultrasonic disperse obtains graphene oxide dispersion.
Step (2) organobentonite is to mix bentonite with water 1:10~1:15 in mass ratio, and swelling is added
The cetyl dimethyl ammonium bromide and 0.1~0.2 times of bentonite quality of caprolactam that 0.1~0.2 times of soil property amount, stirring are anti-
Ying Hou is filtered, dry, and grinding obtains organobentonite.
Step (3) initiator is potassium peroxydisulfate, any one in ammonium persulfate or sodium peroxydisulfate.
Step (3) described catalyst is any one in sulfuric acid or dicyclohexylcarbodiimide that mass fraction is 70~85%
Kind.
Step (4) coupling agent is any one in phthalate ester coupling agent or aluminate coupling agent.
Step (4) dispersing agent is dispersing agent NNO, any one in Dispersant MF or dispersing agent 5040.
The beneficial effects of the present invention are:
(1) modified alta-mud is added when preparing conducting polypropylene fiber in the present invention, firstly, bentonite is after modification, stone
Black alkene enters in bentonitic lamellar structure, thus the electric conductivity of product can be made to improve after being added in product, also, due to
In modified alta-mud bentonite with graphene compound tense, first pass through organic intercalation processing, to make bentonite in polypropylene
Dispersibility improve, and then improve the electric conductivity of product;Secondly, the graphene surface contained in modified alta-mud has amino
Group can react in product preparation process with the oxygen-containing group that surface of graphene oxide is added after being added in product,
To form conductive network in interiors of products, and then further increase the electric conductivity of product, mechanical property improves;
(2) modification of nylon 6 is added when preparing conducting polypropylene fiber by the present invention, on the one hand, modification of nylon 6 can be in graphite oxide
It is scattered in polypropylene under the solubilization of alkene, and due to containing evenly dispersed expanded graphite inside modification of nylon 6, thus
Expanded graphite can be made to be uniformly distributed in products, and then further increase the electric conductivity of product, on the other hand, due to oxidation
The characteristic that graphene keeps modification of nylon 6 solubilized in polypropylene more connects so as to form modification of nylon 6 in polypropylene
Continuous club shaped structure, and form more abundant three-dimensional network in the product with modified alta-mud, make the electric conductivity of product into
One step improves.
Specific embodiment
Bentonite is mixed with water 1:10~1:15 in mass ratio, and bentonite is added into the mixture of bentonite and water
The cetyl dimethyl ammonium bromide and 0.1~0.2 times of bentonite quality of caprolactam that 0.1~0.2 times of quality be in temperature
50~75 DEG C, under conditions of revolving speed is 300~350r/min, after being stirred to react 3~5h, filtering obtains organobentonite blank, will
Under conditions of organobentonite blank is 80~90 DEG C in temperature after dry 1~2h, the organobentonite blank after drying is ground
1~2h is ground, organobentonite is obtained;Graphene oxide dispersion is mixed with ethylenediamine 10:1~15:1 in mass ratio, in temperature
It is 60~85 DEG C, under conditions of revolving speed is 300~400r/min, after being stirred to react 3~4h, filtering obtains modified graphene blank,
After modified graphene blank is washed with deionized 5~10 times, and dry 50 under conditions of being 80~90 DEG C in temperature~
80min obtains modified graphene after the modified graphene blank after drying is ground 50~60min;Modified graphene and water are pressed
Mass ratio 1:100~1:180 mixing obtains modified stone under conditions of frequency is 45~55kHz after 30~40min of ultrasonic disperse
Black alkene dispersion liquid mixes modified graphene dispersion liquid with organobentonite 10:1~12:1 in mass ratio, in frequency be 100~
Under the microwave condition of 1000W, after 2~3h of oscillating reactions, filtering obtains filter cake, by filter cake under conditions of temperature is 55~65 DEG C
After dry 2~3h, and the filter cake after drying is ground into 30~50min, obtains modified alta-mud;Expanded graphite and caprolactam are pressed
Mass ratio 2:1~3:1 is mixed in flask, and 10~15 times of expanded graphite quality of N, N- dimethyl formyl are added into flask
Amine, the initiator and 0.1~0.2 times of expanded graphite quality of catalyst of 0.1~0.2 times of expanded graphite quality quality, in temperature
It is 65~85 DEG C, under conditions of revolving speed is 300~350r/min, after being stirred to react 5~8h, filtering obtains pretreatment expanded graphite
Blank must pre-process expansion stone under conditions of being 70~80 DEG C in temperature by pretreatment expanded graphite blank after dry 1~2h
Expanded graphite and the 1:15~1:20 in mass ratio of nylon 6 are mixed in double screw extruder by ink, in temperature be 150~180 DEG C
Under conditions of extruding pelletization, obtain modification of nylon 6;According to parts by weight, it successively weighs: 40~50 parts of polypropylene agglomerates, 10~15
Part 6,5~8 parts of graphene oxides of modification of nylon, 10~12 parts of modified alta-muds, 3~5 parts of coupling agents, 4~6 parts of dispersing agents and 2
~4 parts of dicyclohexyl carbon Asia diamines;Polypropylene agglomerate and modification of nylon 6 are mixed in batch mixer, and are added into batch mixer
Graphene oxide, modified alta-mud, coupling agent, dispersing agent and dicyclohexyl carbon Asia diamines, in temperature be 160~180 DEG C, revolving speed
Under conditions of 260~300r/min, after being stirred 1~2h, obtain blank, blank squeezed out in spinning machine, spinneret to get
Conducting polypropylene fiber.The graphene oxide dispersion is to mix graphene oxide and water 1:100~1:200 in mass ratio
It closes, ultrasonic disperse obtains graphene oxide dispersion.The initiator is potassium peroxydisulfate, any in ammonium persulfate or sodium peroxydisulfate
It is a kind of.The catalyst is any one in sulfuric acid or dicyclohexylcarbodiimide that mass fraction is 70~85%.The coupling
Agent is any one in phthalate ester coupling agent or aluminate coupling agent.The dispersing agent is dispersing agent NNO, Dispersant MF or dispersion
Any one in agent 5040.
Bentonite is mixed with water 1:15 in mass ratio, and bentonite quality is added into the mixture of bentonite and water
0.2 times of cetyl dimethyl ammonium bromide and 0.2 times of bentonite quality of caprolactam are 75 DEG C in temperature, and revolving speed is
Under conditions of 350r/min, after being stirred to react 5h, filtering obtains organobentonite blank, is in temperature by organobentonite blank
Under conditions of 90 DEG C after dry 2h, the organobentonite blank after drying is ground into 2h, obtains organobentonite;By graphene oxide
Dispersion liquid is mixed with ethylenediamine 15:1 in mass ratio, is 85 DEG C in temperature, under conditions of revolving speed is 400r/min, is stirred to react 4h
Afterwards, filter, obtain modified graphene blank, after modified graphene blank is washed with deionized 10 times, and in temperature be 90 DEG C
Under conditions of dry 80min obtain modified graphene after the modified graphene blank after drying is ground 60min;By modified graphite
Alkene is mixed with water 1:180 in mass ratio, under conditions of frequency is 55kHz after ultrasonic disperse 40min, obtains modified graphene dispersion
Liquid mixes modified graphene dispersion liquid with organobentonite 12:1 in mass ratio, in frequency be 1000W microwave condition under,
After oscillating reactions 3h, filtering obtains filter cake, under conditions of being 65 DEG C in temperature by filter cake after dry 3h, and by the filter cake after drying
50min is ground, modified alta-mud is obtained;Expanded graphite and caprolactam 3:1 in mass ratio are mixed in flask, and into flask
15 times of expanded graphite quality of n,N-Dimethylformamide, the initiator and expansion stone of 0.2 times of expanded graphite quality quality is added
The catalyst of 0.2 times of black quality is 85 DEG C in temperature, and under conditions of revolving speed is 350r/min, after being stirred to react 8h, filtering is obtained
Expanded graphite blank is pre-processed, under conditions of being 80 DEG C in temperature by pretreatment expanded graphite blank after dry 2h, must be pre-processed
Expanded graphite and the 1:20 in mass ratio of nylon 6 are mixed in double screw extruder by expanded graphite, the item for being 180 DEG C in temperature
Extruding pelletization under part obtains modification of nylon 6;According to parts by weight, it successively weighs: 50 parts of polypropylene agglomerates, 15 parts of modification of nylon 6,8
Part graphene oxide, 12 parts of modified alta-muds, 5 parts of coupling agents, 6 parts of dispersing agents and 4 parts of dicyclohexyl carbon Asia diamines;By polypropylene
Master batch and modification of nylon 6 are mixed in batch mixer, and graphene oxide is added into batch mixer, modified alta-mud, coupling agent, point
Powder and dicyclohexyl carbon Asia diamines are 180 DEG C in temperature, under conditions of revolving speed is 300r/min, after being stirred 2h, obtain base
Material, blank is squeezed out in spinning machine, spinneret is to get conducting polypropylene fiber.The graphene oxide dispersion is that will aoxidize
Graphene is mixed with water 1:200 in mass ratio, and ultrasonic disperse obtains graphene oxide dispersion.The initiator is potassium peroxydisulfate.
The catalyst is the sulfuric acid that mass fraction is 85%.The coupling agent is phthalate ester coupling agent.The dispersing agent is dispersing agent
NNO。
Bentonite is mixed with water 1:15 in mass ratio, and bentonite quality is added into the mixture of bentonite and water
0.2 times of cetyl dimethyl ammonium bromide and 0.2 times of bentonite quality of caprolactam are 75 DEG C in temperature, and revolving speed is
Under conditions of 350r/min, after being stirred to react 5h, filtering obtains organobentonite blank, is in temperature by organobentonite blank
Under conditions of 90 DEG C after dry 2h, the organobentonite blank after drying is ground into 2h, obtains organobentonite;By graphene and water
The mixing of 1:180 in mass ratio obtains graphene dispersing solution, by graphite under conditions of frequency is 55kHz after ultrasonic disperse 40min
Alkene dispersion liquid is mixed with organobentonite 12:1 in mass ratio, in frequency be 1000W microwave condition under, after oscillating reactions 3h,
Filtering, obtains filter cake, under conditions of being 65 DEG C in temperature by filter cake after dry 3h, and the filter cake after drying is ground 50min, must changed
Property bentonite;Expanded graphite and caprolactam 3:1 in mass ratio are mixed in flask, and expanded graphite matter is added into flask
The n,N-Dimethylformamide of 15 times of amount, the initiator of 0.2 times of expanded graphite quality quality and 0.2 times of expanded graphite quality urge
Agent is 85 DEG C in temperature, and under conditions of revolving speed is 350r/min, after being stirred to react 8h, filtering must pre-process expanded graphite base
Material obtains pretreatment expanded graphite, will expand stone under conditions of being 80 DEG C in temperature by pretreatment expanded graphite blank after dry 2h
Ink is mixed in double screw extruder with the 1:20 in mass ratio of nylon 6, and extruding pelletization under conditions of being 180 DEG C in temperature must change
Property nylon 6;According to parts by weight, it successively weighs: 50 parts of polypropylene agglomerates, 15 parts of modification of nylon, 6,8 parts of graphene oxides, 12 parts
Modified alta-mud, 5 parts of coupling agents, 6 parts of dispersing agents and 4 parts of dicyclohexyl carbon Asia diamines;Polypropylene agglomerate and modification of nylon 6 are mixed
Together in batch mixer, and graphene oxide is added into batch mixer, modified alta-mud, coupling agent, dispersing agent and dicyclohexyl carbon
Sub- diamines is 180 DEG C in temperature, under conditions of revolving speed is 300r/min, after being stirred 2h, blank is obtained, by blank in spinning
It is squeezed out in machine, spinneret is to get conducting polypropylene fiber.The initiator is potassium peroxydisulfate.The catalyst is that mass fraction is
85% sulfuric acid.The coupling agent is phthalate ester coupling agent.The dispersing agent is dispersing agent NNO.
Bentonite is mixed with water 1:15 in mass ratio, and bentonite quality is added into the mixture of bentonite and water
0.2 times of cetyl dimethyl ammonium bromide and 0.2 times of bentonite quality of caprolactam are 75 DEG C in temperature, and revolving speed is
Under conditions of 350r/min, after being stirred to react 5h, filtering obtains organobentonite blank, is in temperature by organobentonite blank
Under conditions of 90 DEG C after dry 2h, the organobentonite blank after drying is ground into 2h, obtains organobentonite;By graphene oxide
Dispersion liquid is mixed with ethylenediamine 15:1 in mass ratio, is 85 DEG C in temperature, under conditions of revolving speed is 400r/min, is stirred to react 4h
Afterwards, filter, obtain modified graphene blank, after modified graphene blank is washed with deionized 10 times, and in temperature be 90 DEG C
Under conditions of dry 80min obtain modified graphene after the modified graphene blank after drying is ground 60min;By expanded graphite
It is mixed in flask with caprolactam 3:1 in mass ratio, and 15 times of expanded graphite quality of N, N- dimethyl is added into flask
Formamide, the initiator and 0.2 times of expanded graphite quality of catalyst of 0.2 times of expanded graphite quality quality, in temperature be 85 DEG C,
Under conditions of revolving speed is 350r/min, after being stirred to react 8h, filtering must pre-process expanded graphite blank, and pretreatment is expanded stone
Under conditions of black blank is 80 DEG C in temperature after dry 2h, pretreatment expanded graphite is obtained, in mass ratio with nylon 6 by expanded graphite
1:20 is mixed in double screw extruder, and extruding pelletization under conditions of being 180 DEG C in temperature obtains modification of nylon 6;In parts by weight
Meter, successively weighs: 50 parts of polypropylene agglomerates, 15 parts of modification of nylon, 6,8 parts of graphene oxides, 12 parts of bentonites, 5 parts of coupling agents, and 6
Part dispersing agent and 4 parts of dicyclohexyl carbon Asia diamines;Polypropylene agglomerate and modification of nylon 6 are mixed in batch mixer, and to mixing
Graphene oxide, bentonite, coupling agent, dispersing agent and dicyclohexyl carbon Asia diamines are added in machine, in temperature be 180 DEG C, revolving speed
Under conditions of 300r/min, after being stirred 2h, blank is obtained, blank is squeezed out in spinning machine, spinneret is to get conduction poly- third
Alkene fiber.The graphene oxide dispersion is to mix graphene oxide with water 1:200 in mass ratio, and ultrasonic disperse obtains oxygen
Graphite alkene dispersion liquid.The initiator is potassium peroxydisulfate.The catalyst is the sulfuric acid that mass fraction is 85%.The coupling
Agent is phthalate ester coupling agent.The dispersing agent is dispersing agent NNO.
Bentonite is mixed with water 1:15 in mass ratio, and bentonite quality is added into the mixture of bentonite and water
0.2 times of cetyl dimethyl ammonium bromide and 0.2 times of bentonite quality of caprolactam are 75 DEG C in temperature, and revolving speed is
Under conditions of 350r/min, after being stirred to react 5h, filtering obtains organobentonite blank, is in temperature by organobentonite blank
Under conditions of 90 DEG C after dry 2h, the organobentonite blank after drying is ground into 2h, obtains organobentonite;By graphene oxide
Dispersion liquid is mixed with ethylenediamine 15:1 in mass ratio, is 85 DEG C in temperature, under conditions of revolving speed is 400r/min, is stirred to react 4h
Afterwards, filter, obtain modified graphene blank, after modified graphene blank is washed with deionized 10 times, and in temperature be 90 DEG C
Under conditions of dry 80min obtain modified graphene after the modified graphene blank after drying is ground 60min;By modified graphite
Alkene is mixed with water 1:180 in mass ratio, under conditions of frequency is 55kHz after ultrasonic disperse 40min, obtains modified graphene dispersion
Liquid mixes modified graphene dispersion liquid with organobentonite 12:1 in mass ratio, in frequency be 1000W microwave condition under,
After oscillating reactions 3h, filtering obtains filter cake, under conditions of being 65 DEG C in temperature by filter cake after dry 3h, and by the filter cake after drying
50min is ground, modified alta-mud is obtained;According to parts by weight, it successively weighs: 50 parts of polypropylene agglomerates, 15 parts of 6,8 parts of nylon oxidations
Graphene, 12 parts of modified alta-muds, 5 parts of coupling agents, 6 parts of dispersing agents and 4 parts of dicyclohexyl carbon Asia diamines;By polypropylene agglomerate with
Nylon 6 is mixed in batch mixer, and graphene oxide is added into batch mixer, modified alta-mud, coupling agent, dispersing agent and two rings
Hexyl carbon Asia diamines is 180 DEG C in temperature, under conditions of revolving speed is 300r/min, after being stirred 2h, blank is obtained, by blank
It is squeezed out in spinning machine, spinneret is to get conducting polypropylene fiber.The graphene oxide dispersion is by graphene oxide and water
The mixing of 1:200 in mass ratio, ultrasonic disperse obtain graphene oxide dispersion.The initiator is potassium peroxydisulfate.The catalyst
The sulfuric acid for being 85% for mass fraction.The coupling agent is phthalate ester coupling agent.The dispersing agent is dispersing agent NNO.
Comparative example: the conducting polypropylene fiber material of Wuxi material production Co., Ltd production.
Example 1 to the resulting conducting polypropylene fiber of example 4 and comparative example product are subjected to performance detection, specific detection side
Method is as follows:
Mechanical property: the mechanical property of LQ-300KLLY electronic fiber strength tester measurement test specimen is utilized.Test condition: tensile elongation
For 100mm, tensile speed 10mm/min.Every group of test specimen, which stretches 10 times, to be averaged, and breaking strength and introductory die are finally obtained
Amount.
Electric conductivity: the volume resistivity of the fiber using DZ2631 insulation resistance instrument measurement as-spun fibre and after stretching,
Test condition: fiber clamp distance is 5cm, 50~250V of discharge voltage.Every group of fiber is surveyed 10 times, and being averaged for 10 readings is taken
Value.
Specific testing result is as shown in table 1:
1 conducting polypropylene fibre property testing result of table
By 1 testing result of table it is found that the conducting polypropylene fiber of technical solution of the present invention preparation have excellent mechanical property and
The characteristics of electric conductivity, has broad prospects in the development of macromolecule conducting material technology industry.
Claims (7)
1. a kind of preparation method of conducting polypropylene fiber, it is characterised in that specific preparation step are as follows:
(1) graphene oxide dispersion is mixed with ethylenediamine 10:1~15:1 in mass ratio, after being stirred to react, is filtered, washing,
Dry, grinding obtains modified graphene;
(2) modified graphene being mixed with water 1:100~1:180 in mass ratio, ultrasonic disperse obtains modified graphene dispersion liquid,
Modified graphene dispersion liquid is mixed with organobentonite 10:1~12:1 in mass ratio, under microwave condition, after oscillating reactions,
Filtering, dry, grinding obtains modified alta-mud;
(3) expanded graphite is mixed with caprolactam 2:1~3:1 in mass ratio, and is added 10~15 times of expanded graphite quality
N,N-Dimethylformamide, the initiator of 0.1~0.2 times of expanded graphite quality quality and 0.1~0.2 times of expanded graphite quality
Catalyst after being stirred to react, filters, dry, obtains pretreatment expanded graphite, by expanded graphite and the 1:15 in mass ratio of nylon 6~
1:20 mixing, is granulated, obtains modification of nylon 6;
(4) according to parts by weight, it successively weighs: 40~50 parts of polypropylene agglomerates, 10~15 parts of 6,5~8 parts of modification of nylon oxidations
Graphene, 10~12 parts of modified alta-muds, 3~5 parts of coupling agents, 4~6 parts of dispersing agents and 2~4 parts of dicyclohexyl carbon Asia diamines;
Polypropylene agglomerate is mixed with modification of nylon 6, and graphene oxide is added, modified alta-mud, coupling agent, dispersing agent and two hexamethylenes
Base carbon Asia diamines after being stirred, squeezes out, spinneret is to get conducting polypropylene fiber.
2. a kind of preparation method of conducting polypropylene fiber according to claim 1, it is characterised in that: step (1) is described
Graphene oxide dispersion is to mix graphene oxide with water 1:100~1:200 in mass ratio, and ultrasonic disperse obtains oxidation stone
Black alkene dispersion liquid.
3. a kind of preparation method of conducting polypropylene fiber according to claim 1, it is characterised in that: step (2) is described
Organobentonite is to mix bentonite with water 1:10~1:15 in mass ratio, and be added the ten of 0.1~0.2 times of bentonite quality
Six alkyl dimethyl ammonium bromides and 0.1~0.2 times of bentonite quality of caprolactam after being stirred to react, filter, dry, grinding,
Obtain organobentonite.
4. a kind of preparation method of conducting polypropylene fiber according to claim 1, it is characterised in that: step (3) is described
Initiator is potassium peroxydisulfate, any one in ammonium persulfate or sodium peroxydisulfate.
5. a kind of preparation method of conducting polypropylene fiber according to claim 1, it is characterised in that: step (3) is described
Catalyst is any one in sulfuric acid or dicyclohexylcarbodiimide that mass fraction is 70~85%.
6. a kind of preparation method of conducting polypropylene fiber according to claim 1, it is characterised in that: step (4) is described
Coupling agent is any one in phthalate ester coupling agent or aluminate coupling agent.
7. a kind of preparation method of conducting polypropylene fiber according to claim 1, it is characterised in that: step (4) is described
Dispersing agent is dispersing agent NNO, any one in Dispersant MF or dispersing agent 5040.
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| CN117265683A (en) * | 2023-11-20 | 2023-12-22 | 江苏金牛能源设备有限公司 | A kind of bentonite loaded antibacterial agent and its application in antibacterial fiber |
| CN118668319A (en) * | 2024-06-03 | 2024-09-20 | 江苏江山红化纤有限责任公司 | Composite fiber based on graphene and preparation process thereof |
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| CN117265683A (en) * | 2023-11-20 | 2023-12-22 | 江苏金牛能源设备有限公司 | A kind of bentonite loaded antibacterial agent and its application in antibacterial fiber |
| CN117265683B (en) * | 2023-11-20 | 2024-04-09 | 江苏金牛能源设备有限公司 | A bentonite-loaded antibacterial agent and its application in antibacterial fiber |
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