CN107723828A - The preparation method and spinning process of a kind of polymolecularity graphene/composite fibre of nylon 6 - Google Patents
The preparation method and spinning process of a kind of polymolecularity graphene/composite fibre of nylon 6 Download PDFInfo
- Publication number
- CN107723828A CN107723828A CN201710952633.6A CN201710952633A CN107723828A CN 107723828 A CN107723828 A CN 107723828A CN 201710952633 A CN201710952633 A CN 201710952633A CN 107723828 A CN107723828 A CN 107723828A
- Authority
- CN
- China
- Prior art keywords
- graphene
- nylon
- spinning
- temperature
- caprolactam
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
-
- 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
- D01D13/00—Complete machines for producing artificial threads
-
- 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
- D01D5/08—Melt spinning methods
-
- 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
- D01D5/12—Stretch-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
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Artificial Filaments (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention relates to a kind of polymolecularity graphene/composite fibre of nylon 6, it is characterised in that：Using micromechanics stripping method, graphite is peeled off into graphene in caprolactam water solution, form uniform and stable scattered graphene/caprolactam water solution, then with graphene/caprolactam water solution raw material, polymerization obtains polymolecularity graphene/nylon 6, and the composite fibre of graphene/nylon 6 is obtained finally by melt spinning.Program synthesis technique is simple, cost is low, it is uneven to solve the problems, such as that current graphene disperses in the melt of nylon 6, assign the characteristics such as nylon 6 fiber antibacterial, antistatic, far infrared, uvioresistant, and nylon 6/poly conjunction is not influenceed, so as to ensure that nylon 6 has the excellent quality of good fibre forming property and fiber.
Description
Technical field
Patent of the present invention is related to the preparation method and spinning process of a kind of polymolecularity graphene/composite fibre of nylon 6, category
In the manufacturing technology field of chemical fibre.
Background technology
Nylon fibre is to realize industrialized synthetic fibers earliest in the world, and excellent performance, purposes in synthetic fibers
One of extensive kind, it has many excellent performances, is gone rotten except possessing shared corrosion-resistant, resistance to of synthetic fibers, be wet strong
Degree is high, is not afraid of and damages by worms, outside the performance such as hydroscopicity is low, also with intensity height, excellent in abrasion resistance, good, the elongate fiber response rate of elasticity
The advantages that high.With people's growth in the living standard, people are to comfortable, the healthcare function growing interest of textile, to the more of fiber
Functionalization requires more and more stronger, and research, the exploitation of the differential nylon fibre of various functionsization are paid attention to all the more with production.
Graphene is with SP2The Two-dimensional Carbon atomic piece that the carbon atom of hydridization is formed, wherein carbon atom are cellular in six sides.
Because graphene is the carbon atomic layer of monolithic, there is very big specific surface area, the ratio of single-layer graphene is drawn by theoretical calculation
Surface area is 2630m2/ g, this is activated carbon more than twice.Research finds that graphene also has excellent electric property, mainly
Depending on the shape and the number of plies of graphene, graphene also has excellent heat conductivility, and its thermal conductivity factor reaches 3000W/ (m
K), it is heat conductivility is best in addition to metal material.Because graphene has unique nanostructured and excellent items
Can, graphene can be added in polymeric matrix as excellent multi-functional filler, assign matrix excellent performance.Simultaneously with holding high
Expensive CNT is compared, and graphene raw material is easy to get, cheap, and preparation method is also simple and convenient, so it is expected to replace carbon
Nanotube turns into the high quality filler of polymer matrix composite.
At present, the method for preparing graphene/nylon 6 composite mainly has physical blending process and in-situ copolymerization method.Blending method
Refer to nano-particle is added directly into polymeric matrix under mechanical force and mixed, including melt-blending process and molten
Liquid blending method etc., blending method is simple to operate, it is easy to accomplish industrialization, but nano-particle is easily reunited, in polymeric matrix
It is difficult to be uniformly dispersed.In-situ copolymerization method is before nylon polymerization, by graphene dispersion into monomer, then one kind side being polymerize
Method, and current development trend.
The difficult point that graphene/Nylon Nanocomposite of function admirable is prepared mainly realizes function powder in Buddhist nun
Machinability of replacement cycle that is dispersed, extending filament spinning component, raising functional fibre in imperial melt etc..Chinese invention is special
In sharp " injection-class graphite-filled high-temperature nylon and its manufacture craft " (CN102898821A), graphene is divided with mechanical means
It is scattered in nylon, the phenomenon reunited occurs.A kind of Chinese invention patent " preparation side of the graphite oxide nanocomposite of nylon 6/
In method " (CN101760011A), in-situ polymerization is carried out with graphite oxide and caprolactam, nylon 6 is grafted on graphene, from
And by graphene dispersion among nylon 6, but its dispersiveness is not improved.A kind of Chinese invention patent " graphite
In the preparation method of the fiber of alkene modification of nylon 6 " (CN 103215689A), by surface of graphene oxide amination, improving graphite
Interaction between alkene and nylon, the dispersiveness of graphene is improved, graphene modification of nylon fibre property is improved to reach
Effect, but it needs to be acylated graphene, and then reamination, lengthens the whole preparation flow of product, cost also increases, no
Beneficial to industrialized production.
The content of the invention
An object of the present invention is to overcome above-mentioned deficiency, there is provided a kind of polymolecularity graphene/composite fibre of nylon 6
Preparation method.Program synthesis technique is simple, and cost is low, solves current graphene and disperses uneven ask in the melt of nylon 6
Topic, the characteristics such as nylon 6 fiber antibacterial, antistatic, far infrared, uvioresistant are assigned, and do not influence nylon 6/poly conjunction, so as to ensure Buddhist nun
Dragon 6 has the excellent quality of good fibre forming property and fiber.
The second object of the present invention is to provide a kind of spinning process of polymolecularity graphene/composite fibre of nylon 6.
Technical scheme is used by the present invention solves the above problems：A kind of polymolecularity graphene/composite fibre of nylon 6
Preparation method, using micromechanics stripping method, graphite is peeled off into graphene in caprolactam water solution, formed uniform and stable
Scattered graphene/caprolactam water solution, polymolecularity is then obtained with graphene/caprolactam water solution raw material, polymerization
Graphene/nylon 6, the composite fibre of graphene/nylon 6 is obtained finally by melt spinning.
A kind of preparation method of polymolecularity graphene/composite fibre of nylon 6, it is the step of the preparation method：
（1）Graphite is placed in caprolactam water solution, peeled off graphene by micromechanics stripping means, forms stable stone
Black alkene/caprolactam water solution.Containing caprolactam it is 10-80wt% in the caprolactam water solution, the graphene formed/
Caprolactam water solution graphene content accounts for the 0.1-10wt% of caprolactam content, and the exfoliation temperature is 10-60 DEG C, described
Between the planar dimension of graphene is 0.1-10 μm, the number of plies is 1-10 layers.
（2）Will（1）Obtained slurries are placed in pressure to carry out ring-opening reaction under 0.3-5MPa pressure with additive, in this mistake
Cheng Zhong, reaction temperature are 220-300 DEG C, reaction time 1-6h, and key reaction is the hydrolysis of caprolactam, and addition is anti-
Should, while water unnecessary in system is removed；The additive is one or more of adipic acid, acetic acid, terephthalic acid (TPA), is added
Dosage is the 0.01-1wt% relative to quality of caprolactam.
（3）Will（2）Obtained melt, which is placed under normal pressure, to be continued to react.Reaction temperature is 220-280 DEG C, reaction time 3-
8h.Polycondensation reaction of this process key reaction between the oligomer of nylon 6.
（4）, will according to the requirement of final products（3）Obtained melt, which is placed under vacuum environment, to be reacted, pressure 0-
200pa, reaction temperature are 220-280 DEG C, reaction time 0-3h, and this reaction is mainly that the acid amides of the strand of nylon 6 exchanges instead
The process of small molecule and should be removed.
（5）Will（4）Middle obtained melt is after cooling, pelletizing, extraction, drying, then delivers to spinning threadling and carry out melt spinning, obtains
Obtain graphene/nylon fiber.
Main chemical reactions equation is：
（1）Ring-opening reaction
（2）Graft reaction
（3）Addition reaction
（4）Polycondensation reaction
（5）Acid amides exchange reaction
A kind of spinning process of graphene/nylon fiber, the technique of the melt spinning are specially：
The FDY techniques are specially：
Spinning temperature is 240-280 DEG C, and the first draw-off godet speed is 4000-4500m/min, and second spinning reel speed is 5000-
6000m/min, draw ratio are 1.1-1.5 times, and cooling wind-warm syndrome is 15-25 DEG C, wind speed 0.5-1m/s, relative humidity 60%-
90%, obtain fully drawn yarn.
The UDY techniques are specially：
Spinning temperature is 240-280 DEG C, spinning speed 700-1500m/min, and cooling wind-warm syndrome is 20-30 DEG C, wind speed 0.3-1m/
S, relative humidity 60%-80%, obtain non-oriented silk.
The POY techniques are specially：
Spinning temperature is 240-280 DEG C, spinning speed 4000-4500m/min, and cooling wind-warm syndrome is 15-25 DEG C, wind speed 0.3-
0.6m/s, relative humidity 60%-80%, obtains preoriented yarn.
The HOY techniques are specially：
Spinning temperature is 240-280 DEG C, spinning speed 4500-6000m/min, and cooling wind-warm syndrome is 15-20 DEG C, wind speed 0.3-
0.5m/s, relative humidity 80%-90%, obtains high oriented yarn.
The BCF techniques are specially：
Spinning temperature is 240-280 DEG C, and cooling wind-warm syndrome is 20-30 DEG C, wind speed 0.3-1m/s, relative humidity 60%-80%, feeding
Roll temperature is 60-120 DEG C, and draw roll temperature is 100-190 DEG C, feeding speed 300-1000m/min, and draw speed is
1000-3500m/min, draw ratio are 3.5-5 times, and deformation hot air temperature is 190-230 DEG C, and air injection pressure is
196kPa-490kPa, winding speed 600-3000m/min, cooling air temperature are 25 DEG C.
Compared with prior art, the advantage of the invention is that：
The present invention uses micromechanics stripping method, peels off graphite into graphene in caprolactam water solution, is formed uniform and stable
Scattered graphene/caprolactam water solution, polymolecularity is then obtained with graphene/caprolactam water solution raw material, polymerization
Graphene/nylon 6, the composite fibre of graphene/nylon 6 is obtained finally by melt spinning.By graphite in caprolactam water solution
Middle realize is peeled off, and can dramatically improve dispersiveness of the graphene in caprolactam.By the ratio for allocating water and caprolactam
The techniques such as example, exfoliation temperature, graphene concentration, wide variation of the graphene in caprolactam content can be achieved.Present invention solution
Current graphene determined in nylon matrix the problem of difficulties in dispersion, technique is simple, is peeled off with graphene, conventional polymerization process base
This is consistent, and greatly remains the performance of each component, imparts the excellent functional performance of nylon 6 fiber.
1）Using micromechanics stripping method, graphite is peeled off into graphene in caprolactam water solution, can be greatly improved
Dispersiveness of the graphene in caprolactam, so as to further increase dispersiveness of the graphene in nylon 6, improve graphite
The utilization ratio of alkene.
2）Using the method for in-situ polymerization, dispersion effect of the graphene in nylon 6 is further increased, so as to improve
Spinnability.
The preparation-obtained composite fibre of graphene/nylon 6 has the functions such as antistatic, far infrared, can take, home textile,
Apply in the fields such as carpet.
Embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments be merely to illustrate the present invention and
It is not used in limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, those skilled in the art
The present invention can be made various changes or modifications, these equivalent form of values equally fall within what the application appended claims were limited
Scope.
Embodiment 1
A kind of preparation method of polymolecularity graphene/composite fibre of nylon 6 is divided into following steps：
（1）Graphite is placed in caprolactam water solution, peeled off graphene by micromechanics stripping means, forms stable stone
Black alkene/caprolactam water solution.Containing caprolactam be 10wt% in the caprolactam water solution, the graphene formed/oneself in
Amide aqueous solution graphene content accounts for the 10wt% of caprolactam content, and the exfoliation temperature is 10 DEG C, the plane of the graphene
Between size is 0.1 μm, the number of plies is 1 layer.
（2）Will（1）Obtained slurries are placed in pressure to carry out ring-opening reaction under 0.3MPa pressure with additive, in this process
In, reaction temperature is 220 DEG C, reaction time 1h, and key reaction is the hydrolysis of caprolactam, addition reaction, simultaneously will
Unnecessary water removes in system；The additive is adipic acid, and addition is the 0.01wt% relative to quality of caprolactam.
（3）Will（2）Obtained melt, which is placed under normal pressure, to be continued to react.Reaction temperature is 220 DEG C, reaction time 3h.This mistake
Polycondensation reaction of the journey key reaction between the oligomer of nylon 6.
（4）, will according to the requirement of final products（3）Obtained melt, which is placed under vacuum environment, to be reacted, pressure 10pa,
Reaction temperature is 220 DEG C, reaction time 0.5h, and this reaction is mainly the acid amides exchange reaction of the strand of nylon 6 and removed small
The process of molecule.
（5）Will（4）Middle obtained melt is after cooling, pelletizing, extraction, drying, then delivers to spinning threadling and carry out melt spinning, obtains
Obtain graphene/nylon fiber.
A kind of spinning process of graphene/nylon fiber as described above, the technique of the melt spinning are specially：
The FDY techniques are specially：
Spinning temperature is 240 DEG C, and the first draw-off godet speed is 4000m/min, and second spinning reel speed is 5000m/min, stretching
Multiple is 1.1 times, and cooling wind-warm syndrome is 15 DEG C, wind speed 0.5m/s, relative humidity 60%, obtains fully drawn yarn；
Embodiment 2
A kind of preparation method of polymolecularity graphene/composite fibre of nylon 6 is divided into following steps：
（1）Graphite is placed in caprolactam water solution, peeled off graphene by micromechanics stripping means, forms stable stone
Black alkene/caprolactam water solution.Containing caprolactam be 80wt% in the caprolactam water solution, the graphene formed/oneself in
Amide aqueous solution graphene content accounts for the 0.1wt% of caprolactam content, and the exfoliation temperature is 60 DEG C, and the graphene is put down
Between face size is 10 μm, the number of plies is 10 layers.
（2）Will（1）Obtained slurries are placed in pressure to carry out ring-opening reaction under 5MPa pressure with additive, in this process
In, reaction temperature is 300 DEG C, reaction time 6h, and key reaction is the hydrolysis of caprolactam, addition reaction, simultaneously will
Unnecessary water removes in system；The additive is acetic acid, and addition is the 1wt% relative to quality of caprolactam.
（3）Will（2）Obtained melt, which is placed under normal pressure, to be continued to react.Reaction temperature is 280 DEG C, reaction time 8h.This mistake
Polycondensation reaction of the journey key reaction between the oligomer of nylon 6.
（4）, will according to the requirement of final products（3）Obtained melt, which is placed under vacuum environment, to be reacted, and pressure is
200pa, reaction temperature are 280 DEG C, reaction time 3h, and this reaction is mainly the acid amides exchange reaction of the strand of nylon 6 and taken off
Except the process of small molecule.
（5）Will（4）Middle obtained melt is after cooling, pelletizing, extraction, drying, then delivers to spinning threadling and carry out melt spinning, obtains
Obtain graphene/nylon fiber.
A kind of spinning process of graphene/nylon fiber as described above, the technique of the melt spinning are specially：
The POY techniques are specially：
Spinning temperature is 280 DEG C, spinning speed 4500m/min, and cooling wind-warm syndrome is 25 DEG C, wind speed 0.6m/s, and relative humidity is
80%, obtain preoriented yarn；
Embodiment 3
A kind of preparation method of polymolecularity graphene/composite fibre of nylon 6 is divided into following steps：
（1）Graphite is placed in caprolactam water solution, peeled off graphene by micromechanics stripping means, forms stable stone
Black alkene/caprolactam water solution.Containing caprolactam be 40wt% in the caprolactam water solution, the graphene formed/oneself in
Amide aqueous solution graphene content accounts for the 50wt% of caprolactam content, and the exfoliation temperature is 20 DEG C, the plane of the graphene
Between size is 5 μm, the number of plies is 5 layers.
（2）Will（1）Obtained slurries are placed in pressure to carry out ring-opening reaction under 2MPa pressure with additive, in this process
In, reaction temperature is 250 DEG C, reaction time 3h, and key reaction is the hydrolysis of caprolactam, addition reaction, simultaneously will
Unnecessary water removes in system；The additive is terephthalic acid (TPA), and addition is the 5wt% relative to quality of caprolactam.
（3）Will（2）Obtained melt, which is placed under normal pressure, to be continued to react.Reaction temperature is 260 DEG C, reaction time 6h.This mistake
Polycondensation reaction of the journey key reaction between the oligomer of nylon 6.
（4）, will according to the requirement of final products（3）Obtained melt, which is placed under vacuum environment, to be reacted, and pressure is
100pa, reaction temperature are 260 DEG C, reaction time 2h, and this reaction is mainly the acid amides exchange reaction of the strand of nylon 6 and taken off
Except the process of small molecule.
（5）Will（4）Middle obtained melt is after cooling, pelletizing, extraction, drying, then delivers to spinning threadling and carry out melt spinning, obtains
Obtain graphene/nylon fiber.
A kind of spinning process of graphene/nylon fiber as described above, the technique of the melt spinning are specially：
The HOY techniques are specially：
Spinning temperature is 260 DEG C, spinning speed 5000m/min, and cooling wind-warm syndrome is 18 DEG C, wind speed 0.4m/s, and relative humidity is
85%, obtain high oriented yarn；
Embodiment 4
A kind of preparation method of polymolecularity graphene/composite fibre of nylon 6 is divided into following steps：
（1）Graphite is placed in caprolactam water solution, peeled off graphene by micromechanics stripping means, forms stable stone
Black alkene/caprolactam water solution.Containing caprolactam be 60wt% in the caprolactam water solution, the graphene formed/oneself in
Amide aqueous solution graphene content accounts for the 6wt% of caprolactam content, and the exfoliation temperature is 30 DEG C, the plane of the graphene
Between size is 7 μm, the number of plies is 8 layers.
（2）Will（1）Obtained slurries are placed in pressure to carry out ring-opening reaction under 3MPa pressure with additive, in this process
In, reaction temperature is 270 DEG C, reaction time 4h, and key reaction is the hydrolysis of caprolactam, addition reaction, simultaneously will
Unnecessary water removes in system；The additive is adipic acid, and addition is the 0.6wt% relative to quality of caprolactam.
（3）Will（2）Obtained melt, which is placed under normal pressure, to be continued to react.Reaction temperature is 260 DEG C, reaction time 4h.This mistake
Polycondensation reaction of the journey key reaction between the oligomer of nylon 6.
（4）, will according to the requirement of final products（3）Obtained melt, which is placed under vacuum environment, to be reacted, and pressure is
150pa, reaction temperature are 245 DEG C, reaction time 2h, and this reaction is mainly the acid amides exchange reaction of the strand of nylon 6 and taken off
Except the process of small molecule.
（5）Will（4）Middle obtained melt is after cooling, pelletizing, extraction, drying, then delivers to spinning threadling and carry out melt spinning, obtains
Obtain graphene/nylon fiber.
A kind of spinning process of graphene/nylon fiber as described above, the technique of the melt spinning are specially：
The BCF techniques are specially：
Spinning temperature is 265 DEG C, and cooling wind-warm syndrome is 25 DEG C, wind speed 0.8m/s, relative humidity 70%, and feeding roll temperature is 80 DEG C,
Draw roll temperature is 150 DEG C, feeding speed 500m/min, draw speed 2000m/min, and draw ratio is 4 times, deformation heat
Air themperature is 200 DEG C, air injection pressure 300kPa, winding speed 1200m/min, and cooling air temperature is 25 DEG C.
Claims (8)
- A kind of 1. preparation method of polymolecularity graphene/composite fibre of nylon 6, it is characterised in that：Using micromechanics stripping method, Graphite is peeled off into graphene in caprolactam water solution, forms uniform and stable scattered graphene/caprolactam water solution, Then with graphene/caprolactam water solution raw material, polymerization obtains polymolecularity graphene/nylon 6, finally by melt spinning Obtain the composite fibre of graphene/nylon 6.
- 2. the preparation method of polymolecularity graphene according to claim 1/composite fibre of nylon 6, it is characterised in that：Institute The method of stating comprises the following steps：（1）Graphite is placed in caprolactam water solution, peeled off graphene by micromechanics stripping means, forms stable stone Black alkene/caprolactam water solution；Containing caprolactam it is 10-80wt% in the caprolactam water solution, the graphene formed/ Caprolactam water solution graphene content accounts for the 0.1-10wt% of caprolactam content；（2）Will（1）Obtained slurries are placed in pressure to carry out ring-opening reaction under 0.3-5MPa pressure with additive, in this process In, reaction temperature is 220-300 DEG C, reaction time 1-6h；The additive is in adipic acid, acetic acid, terephthalic acid (TPA) More than one, addition is the 0.01-1wt% relative to quality of caprolactam；（3）Will（2）Obtained melt, which is placed under normal pressure, to be continued to react, and reaction temperature is 220-280 DEG C, reaction time 3-8h；（4）, will according to the requirement of final products（3）Obtained melt, which is placed under vacuum environment, to be reacted, pressure 0-200pa, Reaction temperature is 220-280 DEG C, reaction time 0-3h；（5）Will（4）Middle obtained melt is after cooling, pelletizing, extraction, drying, then delivers to spinning threadling and carry out melt spinning, obtains stone Black alkene/nylon fiber.
- 3. the preparation method of polymolecularity graphene according to claim 2/composite fibre of nylon 6, it is characterised in that：Institute State step（1）Middle exfoliation temperature is 10-60 DEG C, and between the planar dimension of the graphene is 0.1-10 μm, the number of plies is 1-10 layers.
- A kind of 4. composite fiber spinning method of polymolecularity graphene/nylon 6, it is characterised in that：FDY techniques are specially：Spinning Temperature is 240-280 DEG C, and the first draw-off godet speed is 4000-4500m/min, and second spinning reel speed is 5000-6000m/ Min, draw ratio are 1.1-1.5 times, and cooling wind-warm syndrome is 15-25 DEG C, wind speed 0.5-1m/s, relative humidity 60%-90%, is obtained Fully drawn yarn.
- A kind of 5. composite fiber spinning method of polymolecularity graphene/nylon 6, it is characterised in that：The UDY techniques are specially： Spinning temperature is 240-280 DEG C, spinning speed 700-1500m/min, and cooling wind-warm syndrome is 20-30 DEG C, wind speed 0.3-1m/s, phase It is 60%-80% to humidity, obtains non-oriented silk.
- A kind of 6. composite fiber spinning method of polymolecularity graphene/nylon 6, it is characterised in that：The POY techniques are specially： Spinning temperature is 240-280 DEG C, spinning speed 4000-4500m/min, and cooling wind-warm syndrome is 15-25 DEG C, wind speed 0.3-0.6m/ S, relative humidity 60%-80%, obtains preoriented yarn.
- A kind of 7. composite fiber spinning method of polymolecularity graphene/nylon 6, it is characterised in that：The HOY techniques are specially： Spinning temperature is 240-280 DEG C, spinning speed 4500-6000m/min, and cooling wind-warm syndrome is 15-20 DEG C, wind speed 0.3-0.5m/ S, relative humidity 80%-90%, obtains high oriented yarn.
- A kind of 8. composite fiber spinning method of polymolecularity graphene/nylon 6, it is characterised in that：The BCF techniques are specially： Spinning temperature is 240-280 DEG C, and cooling wind-warm syndrome is 20-30 DEG C, wind speed 0.3-1m/s, relative humidity 60%-80%, feeds roller temperature Spend for 60-120 DEG C, draw roll temperature is 100-190 DEG C, feeding speed 300-1000m/min, draw speed 1000- 3500m/min, draw ratio are 3.5-5 times, and deformation hot air temperature is 190-230 DEG C, air injection pressure 196kPa- 490kPa, winding speed 600-3000m/min, cooling air temperature are 25 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710952633.6A CN107723828A (en) | 2017-10-13 | 2017-10-13 | The preparation method and spinning process of a kind of polymolecularity graphene/composite fibre of nylon 6 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710952633.6A CN107723828A (en) | 2017-10-13 | 2017-10-13 | The preparation method and spinning process of a kind of polymolecularity graphene/composite fibre of nylon 6 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107723828A true CN107723828A (en) | 2018-02-23 |
Family
ID=61211201
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710952633.6A Pending CN107723828A (en) | 2017-10-13 | 2017-10-13 | The preparation method and spinning process of a kind of polymolecularity graphene/composite fibre of nylon 6 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107723828A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108586730A (en) * | 2018-04-27 | 2018-09-28 | 长乐恒申合纤科技有限公司 | A kind of continuous preparation method of graphene nylon chips and products thereof |
| CN108677257A (en) * | 2018-03-22 | 2018-10-19 | 长乐力恒锦纶科技有限公司 | Highly oriented type graphene oxide chinlon 6 filament and its preparation process |
| CN108815553A (en) * | 2018-07-17 | 2018-11-16 | 杭州高烯科技有限公司 | A kind of graphene self-adhering fascia |
| CN109267348A (en) * | 2018-08-31 | 2019-01-25 | 陆海林 | A kind of preparation method and applications of the textile material added with graphene |
| CN109321999A (en) * | 2018-10-17 | 2019-02-12 | 浙江方圆聚合纤有限公司 | A kind of efficient far infrared, 6 fiber of ultraviolet resistant nylon and preparation method thereof |
| CN110511375A (en) * | 2018-05-22 | 2019-11-29 | 上海杰事杰新材料(集团)股份有限公司 | A kind of static resistant polyamide composite material and preparation method |
| CN111155193A (en) * | 2020-01-20 | 2020-05-15 | 福建中锦新材料有限公司 | Synthetic method of fiber-forming polymer |
| CN111909372A (en) * | 2020-06-29 | 2020-11-10 | 宁波石墨烯创新中心有限公司 | Graphene/polyamide composite material and preparation method and application thereof |
| CN116507766A (en) * | 2020-11-23 | 2023-07-28 | 李永雨 | Graphene composite fiber and method for manufacturing same |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104480561A (en) * | 2014-12-12 | 2015-04-01 | 东华大学 | Caprolactam hydrolyzed polymer fibres and spinning method thereof |
| CN105439134A (en) * | 2015-12-30 | 2016-03-30 | 成都新柯力化工科技有限公司 | Stripping agent for preparing graphene through mechanical exfoliation |
| CN105669969A (en) * | 2016-02-01 | 2016-06-15 | 东华大学 | Nylon 6 polymerization method and direct spinning method of melt of polymer obtained with nylon 6 polymerization method |
| WO2017025926A1 (en) * | 2015-08-11 | 2017-02-16 | Graphenest, S.A. | Method and device for production of graphene or graphene-like materials |
| CN106906534A (en) * | 2017-03-07 | 2017-06-30 | 杭州高烯科技有限公司 | A kind of high-strength and high-modulus amount Graphene/nylon 6 fiber and preparation method |
-
2017
- 2017-10-13 CN CN201710952633.6A patent/CN107723828A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104480561A (en) * | 2014-12-12 | 2015-04-01 | 东华大学 | Caprolactam hydrolyzed polymer fibres and spinning method thereof |
| WO2017025926A1 (en) * | 2015-08-11 | 2017-02-16 | Graphenest, S.A. | Method and device for production of graphene or graphene-like materials |
| CN105439134A (en) * | 2015-12-30 | 2016-03-30 | 成都新柯力化工科技有限公司 | Stripping agent for preparing graphene through mechanical exfoliation |
| CN105669969A (en) * | 2016-02-01 | 2016-06-15 | 东华大学 | Nylon 6 polymerization method and direct spinning method of melt of polymer obtained with nylon 6 polymerization method |
| CN106906534A (en) * | 2017-03-07 | 2017-06-30 | 杭州高烯科技有限公司 | A kind of high-strength and high-modulus amount Graphene/nylon 6 fiber and preparation method |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108677257A (en) * | 2018-03-22 | 2018-10-19 | 长乐力恒锦纶科技有限公司 | Highly oriented type graphene oxide chinlon 6 filament and its preparation process |
| CN108586730A (en) * | 2018-04-27 | 2018-09-28 | 长乐恒申合纤科技有限公司 | A kind of continuous preparation method of graphene nylon chips and products thereof |
| CN110511375A (en) * | 2018-05-22 | 2019-11-29 | 上海杰事杰新材料(集团)股份有限公司 | A kind of static resistant polyamide composite material and preparation method |
| CN108815553A (en) * | 2018-07-17 | 2018-11-16 | 杭州高烯科技有限公司 | A kind of graphene self-adhering fascia |
| CN109267348A (en) * | 2018-08-31 | 2019-01-25 | 陆海林 | A kind of preparation method and applications of the textile material added with graphene |
| CN109321999A (en) * | 2018-10-17 | 2019-02-12 | 浙江方圆聚合纤有限公司 | A kind of efficient far infrared, 6 fiber of ultraviolet resistant nylon and preparation method thereof |
| CN111155193A (en) * | 2020-01-20 | 2020-05-15 | 福建中锦新材料有限公司 | Synthetic method of fiber-forming polymer |
| CN111909372A (en) * | 2020-06-29 | 2020-11-10 | 宁波石墨烯创新中心有限公司 | Graphene/polyamide composite material and preparation method and application thereof |
| CN116507766A (en) * | 2020-11-23 | 2023-07-28 | 李永雨 | Graphene composite fiber and method for manufacturing same |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107723828A (en) | The preparation method and spinning process of a kind of polymolecularity graphene/composite fibre of nylon 6 | |
| CN105002595B (en) | Polymer composite function fibers containing partial graphene, and preparation method thereof | |
| CN107385545A (en) | Preparation method and the application of copolyesteramide and its fiber that a kind of graphene oxide is modified | |
| CN110079896B (en) | Silicon carbide nanofiber bundle and preparation method thereof | |
| CN102321934B (en) | Cotton imitation polyester filament with high hygroscopicity and preparation method thereof | |
| CN101316956A (en) | Carbon fiber, process for production of polyacrylonitrile-base precursor fiber for carbon fiber production, and process for production of carbon fiber | |
| CN105063796A (en) | High-molecular composite conductive fiber and preparation method thereof | |
| CN107460559A (en) | A kind of preparation method of graphene polyester fiber | |
| JP7066924B2 (en) | Manufacturing method of modified polyester fiber that is easy to dye | |
| CN103320881B (en) | A kind of device and method of preparing skin-core structure conductive carbon nanotube composite fibre | |
| CN107794591A (en) | A kind of preparation method and spinning process of the Anti-radiation polyester fiber based on mechanical stripping graphene | |
| CN103556451A (en) | Method for compounding functional nanoparticles on surfaces of polymer filaments | |
| CN105803602B (en) | The method that the graphene film twisting method of forming prepares graphene fiber | |
| CN107513151B (en) | Graphene/polyester nanocomposite and preparation method thereof | |
| CN107385542A (en) | Preparation method and the application of nylon compound resin and its fiber that a kind of POSS grafted graphene oxides are modified | |
| CN106238726B (en) | A kind of flexible compound nano-silver thread and preparation method thereof | |
| CN110055623A (en) | A kind of high conductivity nickel carbon nanofiber flexible electrode material and preparation method thereof | |
| CN102776600B (en) | Method for preparing efficient far infrared nylon fibers | |
| CN106400197A (en) | Making method of comfortable polyester filament | |
| CN108727808A (en) | - 6 agglomerate material of polyamide, the fiber and purposes comprising it of graphene modification | |
| CN114687001B (en) | Preparation method and application of directional heat-conducting insulating composite fiber | |
| CN106948170A (en) | A kind of post-processing approach of fibre, obtained modified fibre product and application thereof | |
| CN109321999A (en) | A kind of efficient far infrared, 6 fiber of ultraviolet resistant nylon and preparation method thereof | |
| CN107400232A (en) | A kind of copolyesteramide of carbon nano-tube modification and its preparation method of fiber and application | |
| CN114318664B (en) | Flexible carbon nanofiber membrane with orientation structure and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180223 |