CN107447286A - A kind of preparation method of graphene terylene composite master batch and fiber - Google Patents
A kind of preparation method of graphene terylene composite master batch and fiber Download PDFInfo
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- CN107447286A CN107447286A CN201710716646.3A CN201710716646A CN107447286A CN 107447286 A CN107447286 A CN 107447286A CN 201710716646 A CN201710716646 A CN 201710716646A CN 107447286 A CN107447286 A CN 107447286A
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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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
- 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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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- 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
- D01F6/92—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 polyesters
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- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention discloses a kind of preparation method of graphene terylene composite master batch, comprise the following steps：Graphene inorganic agent is mixed with deionized water, the mass percent of graphene inorganic agent is controlled between 3~10wt%, then the solution of the graphene Han 10~30wt% is added, the graphene powder after processing, is dried for standby by 5~60min of heating stirring using press filtration in a nitrogen environment；Graphene powder is mixed with terylene particle or section by mechanical ball mill, sieving obtains graphene terylene composite master batch.The beneficial effects of the invention are as follows：It is good using graphene dacron master grain character uniformity made from this method, one layer graphene of coated with uniform, gloss is obvious, obtained graphene polyester fiber has the polyester fiber of conduction, anti-electromagnetic wave, antistatic and high-efficiency shielding far infrared characterization, substantially improve the physical and chemical properties of ordinary polyester fiber, so as to widen use range, the field of textiles such as wearable product are can be widely used for.
Description
Technical field
The present invention relates to Material Field, more particularly to the preparation method of a kind of graphene dacron master grain and fiber.
Background technology
Graphene (Graphene) be it is a kind of by carbon atom form hexagon be in honeycomb-patterned ordered arrangement two-dimensional material.
Since single-layer graphene is successfully found by Univ Manchester UK within 2004, the every excellent performance of graphene causes scientific research
Scholar and the extensive concern of industrial quarters.The excellent properties of preferable single-layer graphene mainly include：Up to 2630m2g-1's
Theoretical specific surface area, the thermal conductivity factor of 97.7% optical transmittance, up to 5300W/ (mK), more than 15000cm2/ (V
S) resistivity of normal temperature electron mobility, as little as 10-6 Ω cm, these unique properties cause graphene energy storage,
The various fields such as photoelectric device, gas sensor, composite and photo-thermal treatment have high application value and potentiality.
Graphene composite material is to be added to graphene in other components as filler, and then improves the mechanical property of material
Can, thermal property and electric property.Wherein fiber-base composite materials are a kind of functional materials of great application prospect, and it has
The advantages that spontaneous heating, thermal conductivity high, easy to process, so it has very important effect in fields such as weaving, health cares.
Also occurs the research of some graphene terylene composites at this stage, such as Publication No. CN105200547A hair
Bright patent application discloses a kind of preparation method of graphene terylene nanometer composite fibre, including the compound mother of graphene dacron polyester
The preparation process of grain and the step of the composite master batch is prepared into graphene terylene nanometer composite fibre, using halogenated hydrocarbons, work(
Energyization is modified and modified graphene oxide, then by modified graphene and dacron polyester compound system in double screw extruder
It is standby go out graphene terylene nanometer composite master batch, finally by composite master batch, spinning can be to obtain graphite directly on melt spinning machine
Alkene terylene nanometer composite fibre.But the patent does not carry out specially treated in graphene and dacron polyester to graphene so that
Graphene and the binding ability that dacron polyester is cut into slices are poor, are unfavorable for the uniformity of later stage spinning and the mixing of graphene terylene, shadow
Ring the feature of later product.
The content of the invention
For overcome in the prior art product graphene dacron master grain character uniformity it is poor, the improvement to polyester fiber performance
Very limited, the dispersiveness and compatibility of graphene powder and terylene particle or section are poor, graphene and terylene particle or cut
The problems such as piece binding ability deficiency, the invention provides a kind of preparation method of graphene terylene composite master batch, including such as
Lower step：
Step 1：Graphene processing, graphene inorganic agent is mixed with deionized water, controls the quality of graphene inorganic agent
Then percentage adds the solution of the graphene Han 10~30wt%, in a nitrogen environment heating stirring 5 between 3~10wt%
~60min, the graphene powder after processing is dried for standby using press filtration；
Step 2：Prepared by masterbatch, the graphene powder obtained in step 1 and terylene particle or section are passed through into mechanical ball
Mill mixing, sieving obtain graphene terylene composite master batch.
Graphene powder is handled using graphene inorganic agent and deionized water mixed solution, substitute it is single go from
Sub- water, substantially increase graphene powder surface and terylene particle or the binding ability of section so that terylene particle or section bag
The graphene powder covered is uniformly and firm, effectively improves the feature of polyester fiber material.
Further, graphene inorganic agent described in step 1 is one kind in bromine water, bromine, lodine chloride, IBr, or
Two or more mixtures.
Further, the concentration of the graphene inorganic agent is 5wt%.
Further, the mass fraction of the graphene powder is preferably 15wt%.
Further, ball milling pearl is provided with the mechanical ball mill, the ball milling pearl is the inorganic abrading-ball of 0.5~5 millimeter of diameter.
Further, the material of the inorganic abrading-ball is aluminum oxide or corundum.
Further, the ball milling speed of the mechanical ball mill is 200~350rpm/min, preferably 250rpm/min.
Further, the Ball-milling Time of the mechanical ball mill is 2~12h, preferably 4h.
Present invention also offers a kind of preparation method of graphene polyester fiber, using above-mentioned master batch as raw material, by 1~
20wt% graphite is added in high speed mixer simultaneously with the masterbatch, and spinning manifold is squeezed into through extruder after being well mixed,
Graphene polyester fiber is made by drawing process again.
Further, the spinning speed control of the spinning manifold is controlled 250 in 1100~1200m/min, spinning temperature
~260 DEG C.
Further, the drawing process includes drawing-off and batched, and drawing-off uses oil bath drawing-off and steam drafting twice drawing-off
Technique, at 1.5~2 times, drawing temperature is controlled at 70~80 DEG C for drafting multiple control, and the oil bath that oil bath drawing-off uses is formulated as 20
~30 parts by weight tow smooth agents, 30~40 parts by weight softening agents, 10~18 parts by weight antistatic additive, 5~8 part by weight of hydrophilic
Agent, the crosslinking agent of 3~5 parts by weight, the water of 1300 parts by weight；The drafting multiple of steam drafting is 1.05~1.15, temperature 130
~150 DEG C.
Further, the extruder is provided with six temperature provinces, and the temperature of each temperature province is different, is respectively set to
265 DEG C, 286 DEG C, 274 DEG C, 268 DEG C, 280 DEG C, 269 DEG C, drop temperature is arranged to 275 DEG C；The spinning manifold unloading position
Place is provided with measuring pump, and the rotating speed of measuring pump is 35r/min.
Further, the graphite is crystalline flake graphite, the one or more in micro crystal graphite, expanded graphite.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) graphene dacron master grain character uniformity produced by the present invention is good, one layer graphene of coated with uniform, light
Damp obvious, obtained graphene polyester fiber has the terylene of conduction, anti-electromagnetic wave, antistatic and high-efficiency shielding far infrared characterization
Fiber, the physical and chemical properties of ordinary polyester fiber are substantially improved, so as to widen use range, can be widely used for wearing
Wear the field of textiles such as product；
(2) graphene powder is handled with deionized water mixed solution using graphene inorganic agent, substituted single
Deionized water, substantially increase graphene powder surface and terylene particle or the binding ability of section so that terylene particle is cut
The graphene powder of piece cladding is uniformly and firm, effectively improves the feature of polyester fiber material；
Embodiment
With reference to embodiments, the present invention will be described in further detail.It is it should be appreciated that described herein specific real
Example is applied only to explain the present invention, is not intended to limit the present invention.
Embodiment one：
The present embodiment provides a kind of preparation method of graphene polyester fiber, comprises the following steps that：
Step 1：Graphene processing, first mixes bromine with deionized water so that the mass fraction of graphene inorganic agent exists
10%, liquid quality 10wt% graphene body is then added, under nitrogen atmosphere heating stirring 20min, heating-up temperature to 50
DEG C, after the completion of stirring, most of liquid is reclaimed by press filtration.Graphene after processing is dried for standby.
Step 2：Prepared by masterbatch, the graphene powder after step 1 is handled passes through mechanical ball with terylene particle or section
Mill mixing, sieving obtains graphene-terylene composite master batch, while reclaims unnecessary graphene powder, and rotational speed of ball-mill is
200rpm/min, ball milling 12h；
Step 3：Spinning, by 10wt% expanded graphite with obtaining masterbatch into appropriate step 2 while being added at a high speed
In batch mixer, after being well mixed, extruded machine squeezes into spinning manifold, then graphene polyester fiber is made by drawing process.
Embodiment two：
The present embodiment provides a kind of preparation method of graphene polyester fiber, comprises the following steps that：
Step 1：Graphene processing, first mixes bromine water with deionized water so that the mass fraction of graphene inorganic agent exists
3%, liquid quality 30wt% graphene body is then added, under nitrogen atmosphere heating stirring 60min, heating-up temperature to 40
DEG C, after the completion of stirring, most of liquid is reclaimed by press filtration.Graphene after processing is dried for standby.
Step 2：Prepared by masterbatch, the graphene powder after step 1 is handled passes through mechanical ball with terylene particle or section
Mill mixing, sieving obtains graphene-terylene composite master batch, while reclaims unnecessary graphene powder, and rotational speed of ball-mill is
250rpm/min, ball milling 8h；
Step 3：Spinning, by 20wt% crystalline flake graphite with obtaining masterbatch into appropriate step 2 while being added at a high speed
In batch mixer, after being well mixed, extruded machine squeezes into spinning manifold, then graphene polyester fiber is made by drawing process.
Embodiment three：
The present embodiment provides a kind of preparation method of graphene polyester fiber, comprises the following steps that：
Step 1：Graphene processing, first mixes lodine chloride with deionized water so that the mass fraction of graphene inorganic agent
5%, liquid quality 20wt% graphene body is then added, under nitrogen atmosphere heating stirring 60min, heating-up temperature to 30
DEG C, after the completion of stirring, most of liquid is reclaimed by press filtration.Graphene after processing is dried for standby.
Step 2：Prepared by masterbatch, the graphene powder after step 1 is handled passes through mechanical ball with terylene particle or section
Mill mixing, sieving obtains graphene-terylene composite master batch, while reclaims unnecessary graphene powder, and rotational speed of ball-mill is
300rpm/min, ball milling 4h；
Step 3：Spinning, by 1wt% micro crystal graphite with obtaining masterbatch into appropriate step 2 while being added to mixed at a high speed
In material machine, after being well mixed, extruded machine squeezes into spinning manifold, then graphene polyester fiber is made by drawing process.
Example IV：
The present embodiment provides a kind of preparation method of graphene polyester fiber, comprises the following steps that：
Step 1：Graphene processing, first mixes IBr with deionized water so that the mass fraction of graphene inorganic agent
8%, liquid quality 15wt% graphene body is then added, under nitrogen atmosphere heating stirring 40min, heating-up temperature to 50
DEG C, after the completion of stirring, most of liquid is reclaimed by press filtration.Graphene after processing is dried for standby.
Step 2：Prepared by masterbatch, the graphene powder after step 1 is handled passes through mechanical ball with terylene particle or section
Mill mixing, sieving obtains graphene-terylene composite master batch, while reclaims unnecessary graphene powder, and rotational speed of ball-mill is
200rpm/min, ball milling 10h；
Step 3：Spinning, by 10wt% expanded graphite with obtaining masterbatch into appropriate step 2 while being added at a high speed
In batch mixer, after being well mixed, extruded machine squeezes into spinning manifold, then graphene polyester fiber is made by drawing process.
Embodiment five：
The present embodiment provides a kind of preparation method of graphene polyester fiber, comprises the following steps that：
Step 1：Graphene processing, first mixes bromine with deionized water so that the mass fraction of graphene inorganic agent exists
5%, liquid quality 30wt% graphene body is then added, under nitrogen atmosphere heating stirring 30min, heating-up temperature to 50
DEG C, after the completion of stirring, most of liquid is reclaimed by press filtration.Graphene after processing is dried for standby.
Step 2：Prepared by masterbatch, the graphene powder after step 1 is handled passes through mechanical ball with terylene particle or section
Mill mixing, sieving obtains graphene-terylene composite master batch, while reclaims unnecessary graphene powder, and rotational speed of ball-mill is
250rpm/min, ball milling 12h；
Step 3：Spinning, by 15wt% expanded graphite with obtaining masterbatch into appropriate step 2 while being added at a high speed
In batch mixer, after being well mixed, extruded machine squeezes into spinning manifold, then graphene polyester fiber is made by drawing process.
Embodiment six：
The present embodiment provides a kind of preparation method of graphene polyester fiber, comprises the following steps that：
Step 1：Graphene processing, first mixes bromine with deionized water so that the mass fraction of graphene inorganic agent exists
8%, liquid quality 15wt% graphene body is then added, under nitrogen atmosphere heating stirring 20min, heating-up temperature to 50
DEG C, after the completion of stirring, most of liquid is reclaimed by press filtration.Graphene after processing is dried for standby.
Step 2：Prepared by masterbatch, the graphene powder after step 1 is handled passes through mechanical ball with terylene particle or section
Mill mixing, sieving obtains graphene-terylene composite master batch, while reclaims unnecessary graphene powder, and rotational speed of ball-mill is
250rpm/min, ball milling 12h；
Step 3：Spinning, by 15wt% micro crystal graphite with obtaining masterbatch into appropriate step 2 while being added at a high speed
In batch mixer, after being well mixed, extruded machine squeezes into spinning manifold, then graphene polyester fiber is made by drawing process.
Embodiment seven：
The present embodiment provides a kind of preparation method of graphene polyester fiber, comprises the following steps that：
Step 1：Graphene processing, first mixes bromine with deionized water so that the mass fraction of graphene inorganic agent exists
10%, liquid quality 20wt% graphene body is then added, under nitrogen atmosphere heating stirring 20min, heating-up temperature to 40
DEG C, after the completion of stirring, most of liquid is reclaimed by press filtration.Graphene after processing is dried for standby.
Step 2：Prepared by masterbatch, the graphene powder after step 1 is handled passes through mechanical ball with terylene particle or section
Mill mixing, sieving obtains graphene-terylene composite master batch, while reclaims unnecessary graphene powder, and rotational speed of ball-mill is
300rpm/min, ball milling 8h；
Step 3：Spinning, by 5wt% expanded graphite with obtaining masterbatch into appropriate step 2 while being added to mixed at a high speed
In material machine, after being well mixed, extruded machine squeezes into spinning manifold, then graphene polyester fiber is made by drawing process.
Embodiment eight：
The present embodiment provides a kind of preparation method of graphene polyester fiber, comprises the following steps that：
Step 1：Graphene processing, first mixes lodine chloride with deionized water so that the mass fraction of graphene inorganic agent
8%, liquid quality 20wt% graphene body is then added, under nitrogen atmosphere heating stirring 30min, heating-up temperature to 50
DEG C, after the completion of stirring, most of liquid is reclaimed by press filtration.Graphene after processing is dried for standby.
Step 2：Prepared by masterbatch, the graphene powder after step 1 is handled passes through mechanical ball with terylene particle or section
Mill mixing, sieving obtains graphene-terylene composite master batch, while reclaims unnecessary graphene powder, and rotational speed of ball-mill is
200rpm/min, ball milling 12h；
Step 3：Spinning, by 20wt% expanded graphite with obtaining masterbatch into appropriate step 2 while being added at a high speed
In batch mixer, after being well mixed, extruded machine squeezes into spinning manifold, then graphene polyester fiber is made by drawing process.
Comparative example one：
The present embodiment provides a kind of preparation method of graphene polyester fiber, comprises the following steps that：
Step 1：Graphene processing, liquid quality 30wt% graphene body is added in deionized water, in nitrogen atmosphere
Lower heating stirring 60min, heating-up temperature is to 40 DEG C, and after the completion of stirring, most of liquid is reclaimed by press filtration.By the stone after processing
Black alkene is dried for standby.
Step 2：Prepared by masterbatch, the graphene powder after step 1 is handled passes through mechanical ball with terylene particle or section
Mill mixing, sieving obtains graphene-terylene composite master batch, while reclaims unnecessary graphene powder, and rotational speed of ball-mill is
250rpm/min, ball milling 8h；
Step 3：Spinning, by 20wt% crystalline flake graphite with obtaining masterbatch into appropriate step 2 while being added at a high speed
In batch mixer, after being well mixed, extruded machine squeezes into spinning manifold, then graphene polyester fiber is made by drawing process.
Comparative example two：
The present embodiment provides a kind of preparation method of graphene polyester fiber, comprises the following steps that：
Step 1：Graphene processing, first mixes bromine water with deionized water so that the mass fraction of graphene inorganic agent exists
1%, liquid quality 30wt% graphene body is then added, under nitrogen atmosphere heating stirring 60min, heating-up temperature to 40
DEG C, after the completion of stirring, most of liquid is reclaimed by press filtration.Graphene after processing is dried for standby.
Step 2：Prepared by masterbatch, the graphene powder after step 1 is handled passes through mechanical ball with terylene particle or section
Mill mixing, sieving obtains graphene-terylene composite master batch, while reclaims unnecessary graphene powder, and rotational speed of ball-mill is
250rpm/min, ball milling 8h；
Step 3：Spinning, by 20wt% crystalline flake graphite with obtaining masterbatch into appropriate step 2 while being added at a high speed
In batch mixer, after being well mixed, extruded machine squeezes into spinning manifold, then graphene polyester fiber is made by drawing process.
Comparative example three：
The present embodiment provides a kind of preparation method of graphene polyester fiber, comprises the following steps that：
Step 1：Graphene processing, first mixes bromine with deionized water so that the mass fraction of graphene inorganic agent exists
12%, liquid quality 10wt% graphene body is then added, under nitrogen atmosphere heating stirring 20min, heating-up temperature to 50
DEG C, after the completion of stirring, most of liquid is reclaimed by press filtration.Graphene after processing is dried for standby.
Step 2：Prepared by masterbatch, the graphene powder after step 1 is handled passes through mechanical ball with terylene particle or section
Mill mixing, sieving obtains graphene-terylene composite master batch, while reclaims unnecessary graphene powder, and rotational speed of ball-mill is
200rpm/min, ball milling 12h；
Step 3：Spinning, by 10wt% expanded graphite with obtaining masterbatch into appropriate step 2 while being added at a high speed
In batch mixer, after being well mixed, extruded machine squeezes into spinning manifold, then graphene polyester fiber is made by drawing process.
Comparative example four：
The present embodiment provides a kind of preparation method of graphene polyester fiber, comprises the following steps that：
Step 1：Graphene processing, first mixes lodine chloride with deionized water so that the mass fraction of graphene inorganic agent
5%, liquid quality 20wt% graphene body is then added, under nitrogen atmosphere heating stirring 60min, heating-up temperature to 30
DEG C, after the completion of stirring, most of liquid is reclaimed by press filtration.Graphene after processing is dried for standby.
Step 2：Prepared by masterbatch, the graphene powder after step 1 is handled passes through mechanical ball with terylene particle or section
Mill mixing, sieving obtains graphene-terylene composite master batch, while reclaims unnecessary graphene powder, and rotational speed of ball-mill is
300rpm/min, ball milling 4h；
Step 3：Spinning, it is added to masterbatch is obtained in step 2 in high speed mixer, after being well mixed, extruded machine
Spinning manifold is squeezed into, then graphene polyester fiber is made by drawing process.
Comparative example five：
The present embodiment provides a kind of preparation method of graphene polyester fiber, comprises the following steps that：
Step 1：Graphene processing, first mixes bromine water with deionized water so that the mass fraction of graphene inorganic agent exists
3%, liquid quality 30wt% graphene body is then added, under nitrogen atmosphere heating stirring 60min, heating-up temperature to 40
DEG C, after the completion of stirring, most of liquid is reclaimed by press filtration.Graphene after processing is dried for standby.
Step 2：Prepared by masterbatch, the graphene powder after step 1 is handled passes through mechanical ball with terylene particle or section
Mill mixing, sieving obtains graphene-terylene composite master batch, while reclaims unnecessary graphene powder, and rotational speed of ball-mill is
250rpm/min, ball milling 8h；
Step 3：Spinning, by 25wt% expanded graphite with obtaining masterbatch into appropriate step 2 while being added at a high speed
In batch mixer, after being well mixed, extruded machine squeezes into spinning manifold, then graphene polyester fiber is made by drawing process.
Comparative example six：
The present embodiment provides a kind of preparation method of graphene polyester fiber, comprises the following steps that：
Step 1：Graphene processing, first mixes bromine with deionized water so that the mass fraction of graphene inorganic agent exists
10%, liquid quality 10wt% graphene body is then added, under nitrogen atmosphere heating stirring 20min, heating-up temperature to 50
DEG C, after the completion of stirring, most of liquid is reclaimed by press filtration.Graphene after processing is dried for standby.
Step 2：Prepared by masterbatch, the graphene powder after step 1 is handled passes through mechanical ball with terylene particle or section
Mill mixing, sieving obtains graphene-terylene composite master batch, while reclaims unnecessary graphene powder, and rotational speed of ball-mill is
150rpm/min, ball milling 10h；
Step 3：Spinning, by 10wt% expanded graphite with obtaining masterbatch into appropriate step 2 while being added at a high speed
In batch mixer, after being well mixed, extruded machine squeezes into spinning manifold, then graphene polyester fiber is made by drawing process.
Comparative example seven：
The present embodiment provides a kind of preparation method of graphene polyester fiber, comprises the following steps that：
Step 1：Graphene processing, first mixes bromine with deionized water so that the mass fraction of graphene inorganic agent exists
10%, liquid quality 10wt% graphene body is then added, under nitrogen atmosphere heating stirring 20min, heating-up temperature to 50
DEG C, after the completion of stirring, most of liquid is reclaimed by press filtration.Graphene after processing is dried for standby.
Step 2：Prepared by masterbatch, the graphene powder after step 1 is handled passes through mechanical ball with terylene particle or section
Mill mixing, sieving obtains graphene-terylene composite master batch, while reclaims unnecessary graphene powder, and rotational speed of ball-mill is
150rpm/min, ball milling 15h；
Step 3：Spinning, by 10wt% expanded graphite with obtaining masterbatch into appropriate step 2 while being added at a high speed
In batch mixer, after being well mixed, extruded machine squeezes into spinning manifold, then graphene polyester fiber is made by drawing process.
Comparative example eight：
The present embodiment provides a kind of preparation method of graphene polyester fiber, comprises the following steps that：
Step 1：Graphene processing, first mixes lodine chloride with deionized water so that the mass fraction of graphene inorganic agent
5%, liquid quality 20wt% graphene body is then added, under nitrogen atmosphere heating stirring 60min, heating-up temperature to 30
DEG C, after the completion of stirring, most of liquid is reclaimed by press filtration.Graphene after processing is dried for standby.
Step 2：Prepared by masterbatch, the graphene powder after step 1 is handled passes through mechanical ball with terylene particle or section
Mill mixing, sieving obtains graphene-terylene composite master batch, while reclaims unnecessary graphene powder, and rotational speed of ball-mill is
350rpm/min, ball milling 4h；
Step 3：Spinning, by 1wt% micro crystal graphite with obtaining masterbatch into appropriate step 2 while being added to mixed at a high speed
In material machine, after being well mixed, extruded machine squeezes into spinning manifold, then graphene polyester fiber is made by drawing process.
Comparative example nine：
The present embodiment provides a kind of preparation method of graphene polyester fiber, comprises the following steps that：
Step 1：Graphene processing, first mixes lodine chloride with deionized water so that the mass fraction of graphene inorganic agent
5%, liquid quality 20wt% graphene body is then added, under nitrogen atmosphere heating stirring 60min, heating-up temperature to 30
DEG C, after the completion of stirring, most of liquid is reclaimed by press filtration.Graphene after processing is dried for standby.
Step 2：Prepared by masterbatch, the graphene powder after step 1 is handled passes through mechanical ball with terylene particle or section
Mill mixing, sieving obtains graphene-terylene composite master batch, while reclaims unnecessary graphene powder, and rotational speed of ball-mill is
200rpm/min, ball milling 4h；
Step 3：Spinning, by 1wt% micro crystal graphite with obtaining masterbatch into appropriate step 2 while being added to mixed at a high speed
In material machine, after being well mixed, extruded machine squeezes into spinning manifold, then graphene polyester fiber is made by drawing process.
The polyester fiber that the fiber and common process obtained to above-mentioned eight groups of embodiments, nine groups of comparative examples obtains carries out strong
Degree, electric conductivity, ESEM sweep test, obtain following result：
As can be seen from the table, the surface smoothness for the graphene polyester fiber that embodiment one to nine obtains, electric conductivity
And the several performance indications of fibrous fracture strength are integrally better than comparative example one to nine, and its electric conductivity is better than conventional polyester fibre
Dimension.
Comparative example one, two is very few without addition graphene inorganic agent or graphene inorganic agent addition, its fibrous inside stone
The combination defective tightness of black alkene and terylene, so as to cause graphene powder after washing to come off or offset in fibrous inside,
Cause fiber surface roughening, and its ultimate strength will also be less than the fiber product in embodiment；Added in comparative example three
Excessive graphene inorganic agent, is destroyed graphene powder surface characteristic, obtained fiber has intensity difference, not wash resistant etc.
Problem；Graphite is not added in spinning technique in comparative example four, the ultimate strength after being washed on graphene has certain influence, and
And it can also influence its electric conductivity；Excessive graphite is added in comparative example five, this can influence the light of fiber surface after its washing
Sliding effect, and also have considerable influence to the ultimate strength of fiber in itself；Comparative example six to nine be mechanical ball mill technological design not
Rationally, graphene powder is caused can not to be sufficiently mixed with terylene particle or section under identical size, rotating speed is too fast to cause stone
Black alkene powder internal structure is destroyed, and rotating speed then reduces production efficiency slowly excessively, and the control of Ball-milling Time mainly influences ball
Effect is ground, Ball-milling Time is long, can influence production efficiency, and Ball-milling Time is too short, can not complete ball milling；Excessive ball milling can be led
There is fatigue in the fibrous inside for causing to obtain, influences its mechanical property, ball milling deficiency can then make fiber surface coarse, particularly wash
Wash rear obvious, and due to fibrous inside graphene and terylene irrational distribution, also have impact on its mechanical property.
The preferred embodiments of the present invention have shown and described in described above, as previously described, it should be understood that the present invention is not office
Be limited to form disclosed herein, be not to be taken as the exclusion to other embodiment, and available for various other combinations, modification and
Environment, and can be changed in the scope of the invention is set forth herein by the technology or knowledge of above-mentioned teaching or association area
It is dynamic., then all should be appended by the present invention and the change and change that those skilled in the art are carried out do not depart from the spirit and scope of the present invention
In scope of the claims.
Claims (10)
1. a kind of preparation method of graphene terylene composite master batch, it is characterised in that comprise the following steps：
Step 1：Graphene processing, graphene inorganic agent is mixed with deionized water, controls the quality percentage of graphene inorganic agent
Than between 3~10wt%, then add the solution of the graphene Han 10~30wt%, in a nitrogen environment heating stirring 5~
60min, the graphene powder after processing is dried for standby using press filtration；
Step 2：Prepared by masterbatch, the graphene powder obtained in step 1 and terylene particle or section are mixed by mechanical ball mill
Close, sieving obtains graphene terylene composite master batch；
A kind of 2. preparation method of graphene terylene composite master batch according to claim 1, it is characterised in that step
Graphene inorganic agent described in one is one kind in bromine water, bromine, lodine chloride, IBr, or two or more mixtures.
3. the preparation method of a kind of graphene terylene composite master batch according to claim 1, it is characterised in that described
The concentration of graphene inorganic agent is 5wt%.
4. the preparation method of a kind of graphene terylene composite master batch according to claim 1, it is characterised in that described
The mass fraction of graphene powder is preferably 15wt%.
5. the preparation method of a kind of graphene terylene composite master batch according to claim 1, it is characterised in that described
Ball milling pearl is provided with mechanical ball mill, the ball milling pearl is the inorganic abrading-ball of 0.5~5 millimeter of diameter.
6. the preparation method of a kind of graphene terylene composite master batch according to claim 5, it is characterised in that described
The material of inorganic abrading-ball is aluminum oxide or corundum.
7. the preparation method of a kind of graphene terylene composite master batch according to claim 6, it is characterised in that described
The ball milling speed of mechanical ball mill is 200~350rpm/min, preferably 250rpm/min.
8. the preparation method of a kind of graphene terylene composite master batch according to claim 7, it is characterised in that described
The Ball-milling Time of mechanical ball mill is 2~12h, preferably 4h.
9. a kind of preparation method of graphene polyester fiber, it is characterised in that using the master batch as described in claim any one of 1-8
As raw material, 1~20wt% graphite and the masterbatch are added in high speed mixer simultaneously, through extruder after being well mixed
Spinning manifold is squeezed into, then graphene polyester fiber is made by drawing process.
10. the preparation method of a kind of graphene polyester fiber according to claim 9, it is characterised in that the graphite is
Crystalline flake graphite, the one or more in micro crystal graphite, expanded graphite.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108794999A (en) * | 2018-05-02 | 2018-11-13 | 陕西金瑞烯科技发展有限公司 | A kind of preparation method of graphene terylene composite material master batch and fiber |
| CN109534323A (en) * | 2018-11-21 | 2019-03-29 | 黑龙江科技大学 | A kind of preparation method of the graphene for modified dacron filament fiber |
| CN110305431A (en) * | 2019-08-13 | 2019-10-08 | 上海长园电子材料有限公司 | A kind of method and its application of conduction dispersion resin mixing |
| CN111155199A (en) * | 2020-01-10 | 2020-05-15 | 特烯（厦门）科技有限公司 | Preparation method of graphene composite fiber |
| CN115074857A (en) * | 2022-08-02 | 2022-09-20 | 江苏康溢臣生命科技有限公司 | Cool iodine antibacterial fiber and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108794999A (en) * | 2018-05-02 | 2018-11-13 | 陕西金瑞烯科技发展有限公司 | A kind of preparation method of graphene terylene composite material master batch and fiber |
| CN109534323A (en) * | 2018-11-21 | 2019-03-29 | 黑龙江科技大学 | A kind of preparation method of the graphene for modified dacron filament fiber |
| CN110305431A (en) * | 2019-08-13 | 2019-10-08 | 上海长园电子材料有限公司 | A kind of method and its application of conduction dispersion resin mixing |
| CN111155199A (en) * | 2020-01-10 | 2020-05-15 | 特烯（厦门）科技有限公司 | Preparation method of graphene composite fiber |
| CN115074857A (en) * | 2022-08-02 | 2022-09-20 | 江苏康溢臣生命科技有限公司 | Cool iodine antibacterial fiber and preparation method thereof |
| CN115074857B (en) * | 2022-08-02 | 2023-09-29 | 江苏康溢臣生命科技有限公司 | Cool iodine antibacterial fiber and preparation method thereof |
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Application publication date: 20171208 |