CN107287682A - A kind of stone needle composite fibre of graphene-containing and its preparation method and application - Google Patents
A kind of stone needle composite fibre of graphene-containing and its preparation method and application Download PDFInfo
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- CN107287682A CN107287682A CN201710551686.7A CN201710551686A CN107287682A CN 107287682 A CN107287682 A CN 107287682A CN 201710551686 A CN201710551686 A CN 201710551686A CN 107287682 A CN107287682 A CN 107287682A
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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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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
The invention provides stone needle composite fibre of a kind of graphene-containing and its preparation method and application.A kind of stone needle composite fibre of graphene-containing, is mainly made up of following component：Fiber carrier section, stone needle and grapheme material；The grapheme material be the material with graphene film Rotating fields, including graphene, graphene oxide and with any one in Graphene derivative or at least two combination.The present invention is in the composite fibre that stone needle and fibre section are made, introduce grapheme material, to improve the dispersiveness between stone needle and fiber, while improving intensity, far-infrared functional, thermoelectricity capability and the stability of fiber using a variety of good characteristics of grapheme material.
Description
Technical field
The present invention relates to textile material field, more particularly, to a kind of stone needle composite fibre of graphene-containing and its preparation side
Method and application.
Background technology
In recent years, the continuous improvement lived with people is developed rapidly with science and technology, the weaving of various healthcare functions
Fiber and its products are emerged in multitude, such as negative ion far-infrared fiber, biological magnetic fiber and its product.Using these functional fibres
The clothes being made, with certain health care, physical therapy efficacy, have been widely used at present.Stone needle contains 40 multiple beneficials in people
More than 20 kinds of anti-aging element such as calcium, magnesium, zinc, chromium, strontium, selenium necessary to the trace element and mineral matter, and human body of body.Stone needle
There is unusual energy field, act on human body skin and show that extra-far infrared radiation can be produced, its frequency band is extremely wide, and Far-Infrared Frequency is reachable
Scope is 7~20 μm.Stone needle is that some treatments and health care are reached by microcrystal infra-red and the wave band of pulse, if can be by stone needle
Functional fibre is made in the effective fiber that introduces, it will its is played a role efficacy lastingly.
For example, patent application CN102586923A discloses a kind of stone needle functional fiber and its processing technology, by stone needle work(
Energy master batch and polypropylene fiber grade resins are constituted, and the stone needle functional master batch includes following component, is weight percentage：Stone needle powder
Body additives 1~15%, coupling agent 2.5~9%, dispersant 15~25%, vector resin 52~67%.It is preparing stone needle work(
Can master batch when need to use the coupling agent of wide variety of conventional and dispersant, the dispersant used have PE macromolecule wax, PP molecular wax or
EVA, the coupling agent used has silane, titanate esters, Aluminate and aluminium titanium composite coupler, and these additives can dilute carrier tree
Fat, reduction prepares the intensity of fiber.
Patent application CN105970327A discloses a kind of health care regenerated celulose fibre containing stone needle, and it is by stone needle and again
Raw fiber is constituted, and also added conventional dispersant and thickener, dispersant used have polypropylene sodium salt, many sodium metaphosphates,
Sodium pyrophosphate, zinc stearate, calgon, polyethylene glycol, triethyl group hexyl phosphoric acid, nano titanium oxide, thickening used
Agent is sodium carboxymethylcellulose, and these additives also reduce the intensity of regenerated cellulose script, and dry fracture strength only reaches 2.4
~4.6cN/dtex, warming rate is up to 93%.
In view of this, it is special to propose the present invention.
The content of the invention
The first object of the present invention is the stone needle composite fibre for providing a kind of graphene-containing, described stone needle composite fibre
Solve existing product and introduce the technical problem that fibre strength is reduced after stone needle.
The second object of the present invention is the preparation method for the stone needle composite fibre for providing above-mentioned graphene-containing, described system
Preparation Method flow is simple, process and existing product difference are small, therefore transformation difficulty when reducing product up-gradation to workshop.
The third object of the present invention is the application for the stone needle composite fibre for providing above-mentioned graphene-containing, and it is widely used,
It is mainly used in field of textiles, for example, manufactures yarn, fabric, non-woven fabrics, filtering material or warming wadding suede inserts.
In order to solve the above technical problems, the invention provides following technical scheme：
A kind of stone needle composite fibre of graphene-containing, is mainly made up of following component：Fiber carrier section, stone needle and graphite
Alkene material；
The grapheme material is the material with graphene film Rotating fields, including graphene, graphene oxide and and stone
In black ene derivative any one or at least two combination.
Graphene of the present invention is prepared including graphite by stripping method.Graphene oxide can be prepared by reducing
Obtain, either graphite is prepared by redox or carbonaceous gas is prepared by CVD, or with biomass
Prepared for raw material by high-temperature cracking method.
The present invention introduces grapheme material, to improve stone needle and fiber in the composite fibre that stone needle and fiber are made
Between dispersiveness, while utilize grapheme material high-strength characteristic improve fibre strength.
Specifically principle is the present invention：In the inside of composite fibre, microscopic pattern is shown as：Fiber carrier section, stone needle
Mutually disperse with grapheme material, i.e., stone needle is dispersed in the two-dimensional slice structure of grapheme material, and is coated on graphite
The surface of alkene material, so that the accumulation or reunion that avoid itself ion lead to not be dispersed in fiber, it is also effectively anti-
The reunion of graphite alkenes material is stopped.It can be seen that, in the present invention, graphite alkenes material and stone needle decentralized medium each other were both improved
The function affect of stone needle in the fibre, and improved again using graphite alkenes material good intensity, pliability and focus
Fracture strength, elongation at break and the thermoelectricity capability of condensating fiber.
After testing, the fracture strength of stone needle composite fibre of the invention is not only no because introducing the reduction of the materials such as stone needle,
More than 20%, or even raising 50% can be improved on the contrary, and its far infrared normal emittance can reach more than 0.91, and bacteriostasis rate can reach
More than 90%.
Graphene of the present invention can be commercially available graphene, the graphite that can be also obtained by different preparation methods
Alkene, such as mechanical stripping method, epitaxial growth method, chemical vapor infiltration, graphite oxidation reducing process.But, some methods are difficult
Realization is prepared in the theoretic graphene of stricti jurise, such as graphene that a part of prior art is prepared on a large scale
Can there are some impurity elements, other allotropes of carbon or the non-individual layer of the number of plies even graphene-structured (example of multilayer
Such as 3 layers, 5 layers, 10 layers, 20 layers), the graphene that the present invention is utilized also includes the graphite on above-mentioned non-critical theory of meaning
Alkene.
Graphene oxide of the present invention can be prepared by commercially available graphene oxide or partial reduction crosslinking
Graphene it is oxidized after product, can also be PECVD prepare graphene it is oxidized after product or graphite
Prepared by redox, carbonaceous gas is prepared by CVD or passes through high temperature by raw material of biomass
Cracking process is prepared.
Above stone needle composite fibre can also be improved further, to improve its many performance, for example:
Preferably, by weight, 0.5-3 parts of 100 parts of fiber carrier section, 1-3 parts of stone needle and grapheme material.
Ratio to raw material is carried out after above optimization, can not only be improved the intensity of product, can also be improved its far infrared
Function, especially warming rate.
Similarly, further preferably：1.5-3 parts of 100 parts of fiber carrier section, 1-2 parts of stone needle and grapheme material.
Preferably, the particle diameter of the stone needle is below 1 μm.
The particle diameter of stone needle is excessive to be unfavorable for spinning, can block spinneret orifice or cause fracture of wire, it is considered to this factor, the grain of stone needle
Footpath is preferred below 1 μm.
Preferably, the particle diameter of the grapheme material is below 8 μm.
The excessive easy reunion of particle diameter of grapheme material.In addition, particle diameter is too small or particle diameter excessively concentrates also easily reunion,
Therefore, the particle diameter of grapheme material is preferably separated into different scopes, and such as particle diameter accounts for fraction, 5 μm~8 μm at 1~5 μm
Account for fraction, or show as the lower limit of particle diameter distribution and higher limit differs larger.
Preferably, in the grapheme material quality >=stone needle quality of the particle diameter more than 1 μm 1/4.
Consider the microscopic pattern of grapheme material and stone needle, and change of the spinning technique to particle shape, stone is worked as in discovery
In black alkene material quality >=stone needle quality of the particle diameter more than 1 μm 1/4 when, dispersion effect more preferably, product it is comprehensive
Can be more preferably.
Similarly, further preferably：Total matter of the quality≤stone needle of the particle diameter more than 1 μm in the grapheme material
Amount.
Preferably, the fiber carrier section is selected from polyester fiber, acrylic fiber, nylon fibre, polypropylene fiber and spandex
One or more in one or more in fiber, preferably polyester fiber, acrylic fiber and nylon fibre.
Can after polyester fiber, acrylic fiber, nylon fibre, polypropylene fiber and spandex fibre and stone needle, graphene collocation
Obtain preferable properties of product, especially polyester fiber, acrylic fiber and nylon fibre.
Composite fibre obtained by all of above scheme of the present invention can reach following performance：
The dry fracture strength of the stone needle composite fibre of the graphene-containing can improve more than 20%, or even 50%, for example
The dry fracture strength of the stone needle composite polyester fiber of graphene-containing can reach more than 6.8cN/dtex, and conventional polyester fiber
Dry fracture strength for 4.2cN/dtex or so；The dry fracture strength that the stone needle of the graphene-containing is combined nylon fibre can reach
To more than 7.0cN/dtex, and the dry fracture strength of conventional nylon fibre is 5.2cN/dtex or so.
Preferably, the far infrared normal emittance of the stone needle composite fibre is more than 0.91.
Preferably, the bacteriostasis rate of the stone needle composite fibre is more than 90%.
Preferably, Tourmaline is also contained.
Add after Tourmaline, the far-infrared functional of composite fibre can be improved, and total amount effect at 1-3 parts is more preferable,
I.e.：
By weight, 1-3 parts of 100 parts of fiber carrier section, 1-3 parts of stone needle, 0.5-3 parts of grapheme material and Tourmaline.
Preferably, the particle diameter of the Tourmaline is below 1 μm, preferably 200nm-500nm.
The particle diameter of Tourmaline is excessive to be unfavorable for spinning, can block spinneret orifice or cause fracture of wire.Consider this factor, Tourmaline
Particle diameter be preferred below 1 μm, preferably 200nm-500nm.
Preferably, by weight, gross mass≤5 part of Tourmaline and stone needle.
The total amount that Tourmaline and stone needle are added is excessive, can have a negative impact to spinning, and then reduces the drawing of composite fibre
Stretch performance.
The preparation method of the stone needle composite fibre of above-mentioned graphene-containing, comprises the following steps：
The stone needle, the fiber carrier section of the grapheme material and part are mixed to prepare master batch；
The master batch is mixed into progress spinning with the remaining fiber carrier section.
In the above method, the type for preparing master batch and the fiber carrier section used in spinning can be with identical, can also be different.
Preferably, Tourmaline is additionally added when preparing the master batch, 1-3 parts of Tourmalines are preferably added to, Tourmaline and stone needle
Gross mass preferably≤5 parts.
It is described above, add after Tourmaline, the far-infrared functional of composite fibre can be improved.
Preferably, the grapheme material contain particle diameter more than 1 μm and particle diameter be less than 1 μm.
Preferably, when preparing the master batch, grapheme material of the particle diameter more than 1 μm is mixed with stone needle, mixed
Compound A；Grapheme material of the particle diameter below 1 μm is mixed with fiber carrier section, mixture B is obtained；Again will be described
The mixture A and mixture B is mixed to prepare master batch.
Due to having repellency between different material, therefore stone needle is first coated on big particle diameter graphene periphery, Ji Nengqi
To the effect of dispersed graphite alkene, be conducive to itself disperseing again, and stone needle can be caused to be coated on graphene periphery and form larger particles,
Further prevent the reunion with other graphene particles.
In above step, less than more than 1 μm and 1 μm of grapheme material has overlapping on 1 μm of particle diameter, and the present invention is right
This is simultaneously not particularly limited, i.e., 1 μm of grapheme material can both be mixed with stone needle, can also be mixed with fiber carrier section.
Preferably, Tourmaline is additionally added when preparing the mixture A, 1-3 parts of Tourmalines, Tourmaline and stone needle is preferably added to
Gross mass preferably≤5 parts.
As described above, the composite fibre that the present invention is provided is steady in fracture strength, far-infrared functional, thermoelectricity capability, chemistry
Have outstanding performance, therefore, be widely used in terms of qualitative energy, processability, available for manufacture yarn, fabric, non-woven fabrics, filter material
The textile such as material or warming wadding suede inserts.
To sum up, compared with prior art, invention achieves following technique effect：
(1) mechanical performance of stone needle composite fibre, especially fracture strength, elongation at break etc. are improved.
(2) far-infrared functional of stone needle composite fibre is improved, so as to improve its warming rate and other health-care efficacies.
(3) thermoelectricity capability of stone needle composite fibre is improved.
Embodiment
Technical scheme is clearly and completely described below in conjunction with embodiment, but ability
Field technique personnel will be understood that following described embodiment is a part of embodiment of the invention, rather than whole embodiments,
The present invention is merely to illustrate, and is not construed as limiting the scope of the present invention.Based on the embodiment in the present invention, the common skill in this area
The every other embodiment that art personnel are obtained under the premise of creative work is not made, belongs to the model that the present invention is protected
Enclose.Unreceipted actual conditions person in embodiment, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same or instrument
Unreceipted production firm person, is the conventional products that can be obtained by commercially available purchase.
The type of grapheme material provided by the present invention has：
Graphene A：" the model of Changzhou No.6 Element Material Technology Co., Ltd.'s production：SE1231 " conductive and heat-conductive
Type graphene.
Graphene B：" the model of Changzhou No.6 Element Material Technology Co., Ltd.'s production：SE1430 " reinforced stone
Black alkene series.
Graphene C：Using patent publication No., " cellulose is the side that raw material prepares biomass graphene for CN104724699A
The method of embodiment 1 is made in method ".
Embodiment 1
Below by taking polyester fiber as an example, a kind of stone needle composite polyester fiber of graphene-containing is prepared
Feeding：
100 grams of polyester slice, 2 grams of stone needle (particle diameter distribution be 0.5 μm~1 μm), graphene B (particle diameter distribution 0.5 μm~
3 μm) 1.5 grams, wherein more than 1 μm of graphene B is 0.5 gram.
Prepare master batch：
First grapheme material of the particle diameter more than 1 μm is mixed with stone needle, mixture A is obtained；By particle diameter below 1 μm
Grapheme material is mixed with 1/4 polyester slice, obtains mixture B；Again by mixture A and mixture B Hybrid Heatings, carry out high
Speed is mediated, then through twin-screw blending extrusion, master batch is made in cooling, granulation.
Spinning：
Master batch is mixed with remaining polyester slice, by melt extruded spinning, is being post-processed, is producing composite fibre.
Embodiment 2
It is different from the proportioning for differing only in raw material of embodiment 1, be：
100 grams of polyester slice, 3 grams of stone needle (particle diameter distribution be 0.5 μm~1 μm), graphene B (particle diameter distribution is 0.5 μm~
3 μm) 3 grams, wherein more than 1 μm of graphene B is 1 gram.
Embodiment 3
It is different from the proportioning for differing only in raw material of embodiment 1, be：
100 grams of polyester slice, 1 gram of stone needle (particle diameter distribution be 0.5 μm~1 μm), graphene B (particle diameter distribution is 0.5 μm~
3 μm) 0.5 gram, wherein more than 1 μm of graphene B is 0.25 gram.
Embodiment 4-5
It is different from the model for differing only in graphene of embodiment 1, it is that graphene A (embodiment 4), graphene C (are implemented
Example 5), particle diameter distribution is at 1 μm~8 μm.
Embodiment 6
With embodiment 1 differ only in prepare master batch technique it is relatively simple, be specially：
By stone needle, graphene B and polyester slice while Hybrid Heating, carries out high-speed kneading, then through twin-screw blending extrusion,
Cooling, granulation, are made master batch.
Step be the same as Example 1 afterwards.
Embodiment 7
Different from the particle diameter for differing only in stone needle of embodiment 1, its particle diameter distribution is at 1 μm~3 μm.
Embodiment 8
1 gram of Tourmaline (particle diameter distribution is in 200nm-500nm) is added in raw material with differing only in for embodiment 6, and
And added when preparing mixture A.
Embodiment 9
It is different from the addition for differing only in Tourmaline of embodiment 8, it is 3 grams of Tourmalines.
Comparative example 1
Referring to patent application CN102586923A, concrete technology is as follows：
Percentage composition feeding by weight, particle diameter is less than 2 μm of stone needle particle 10%, silane 5%, PE macromolecule wax 25%,
PP resins 60%.By all of above raw material Hybrid Heating, high-speed kneading is carried out, then through twin-screw blending extrusion, is cooled down, granulation,
Master batch is made.
The polypropylene fiber of 2.5 times of its weight is added into master batch, is mixed, by melt extruded spinning, is located after progress
Reason, produces composite fibre.
Comparative example 2
Difference with embodiment 1 is that stone needle is 10g.
Comparative example 3
Difference with embodiment 1 is that stone needle and graphene B particle diameter are all higher than 5 μm.
Comparative example 4
Conventional polyester fiber, producer is Yangzhou family happiness fiber Co., Ltd.
The composite fibre performance of above-mentioned all embodiments and comparative example is as shown in table 1.
The performance of the different stone needle composite fibres of table 1
Finally it should be noted that：Various embodiments above is merely illustrative of the technical solution of the present invention, rather than its limitations；To the greatest extent
The present invention is described in detail with reference to foregoing embodiments for pipe, it will be understood by those within the art that：Its according to
The technical scheme described in foregoing embodiments can so be modified, or which part or all technical characteristic are entered
Row equivalent substitution；And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention technology
The scope of scheme.
Claims (10)
1. the stone needle composite fibre of a kind of graphene-containing, it is characterised in that be mainly made up of following component：Fiber carrier section,
Stone needle and grapheme material；
The grapheme material is the material with graphene film Rotating fields, including graphene, graphene oxide and and graphene
In derivative any one or at least two combination.
2. the stone needle composite fibre of graphene-containing according to claim 1, it is characterised in that by weight, fiber carrier
0.5-3 parts of 100 parts of section, 1-3 parts of stone needle and grapheme material；
Preferably, by weight, 1.5-3 parts of 100 parts of fiber carrier section, 1-2 parts of stone needle and graphite alkenes material.
3. the stone needle composite fibre of graphene-containing according to claim 1, it is characterised in that the particle diameter of the stone needle is in 1 μ
Below m；
Preferably, the particle diameter of the grapheme material is below 8 μm；
Preferably, in the grapheme material quality >=stone needle quality of the particle diameter more than 1 μm 1/4；
Preferably, in the grapheme material quality≤stone needle of the particle diameter more than 1 μm gross mass.
4. the stone needle composite fibre of graphene-containing according to claim 1, it is characterised in that preferably, the fiber is carried
One or more of the body section in polyester fiber, acrylic fiber, nylon fibre, polypropylene fiber and spandex fibre, preferably gather
One or more in ester fiber, acrylic fiber and nylon fibre.
5. the stone needle composite fibre of graphene-containing according to claim 1, it is characterised in that the stone needle composite fibre
Far infrared normal emittance is more than 0.91；
Preferably, the bacteriostasis rate of the stone needle composite fibre is more than 90%.
6. the stone needle composite fibre of graphene-containing according to claim 1, it is characterised in that also contain Tourmaline；
Preferably, the particle diameter of the Tourmaline is below 1 μm, preferably 200nm-500nm；
Preferably, by weight, 100 parts of fiber carrier section, 1-3 parts of stone needle, 0.5-3 parts of grapheme material and Tourmaline 1-3
Part；
Preferably, by weight, gross mass≤5 part of Tourmaline and stone needle.
7. the preparation method of the stone needle composite fibre of the graphene-containing described in claim any one of 1-5, it is characterised in that including
Following steps：
The stone needle, the fiber carrier section of the grapheme material and part are mixed to prepare master batch；
The master batch is mixed into progress spinning with the remaining fiber carrier section.
8. preparation method according to claim 7, it is characterised in that Tourmaline is additionally added when preparing the master batch, preferably
Adding 1-3 part Tourmalines, the gross mass of Tourmaline and stone needle is preferred≤and 5 parts.
9. preparation method according to claim 7, it is characterised in that the grapheme material contains particle diameter more than 1 μm
And particle diameter be less than 1 μm of particle；
Preferably, when preparing the master batch, grapheme material of the particle diameter more than 1 μm is mixed with stone needle, mixture is obtained
A；Grapheme material of the particle diameter below 1 μm is mixed with fiber carrier section, mixture B is obtained；Again by the mixing
The thing A and mixture B is mixed to prepare master batch；
Preferably, be additionally added Tourmaline when preparing the mixture A, be preferably added to 1-3 parts of Tourmalines, Tourmaline and stone needle it is total
Quality preferably≤5 parts.
10. the application of the stone needle composite fibre of the graphene-containing described in claim any one of 1-6, it is characterised in that for making
Make yarn, fabric, non-woven fabrics, filtering material or warming wadding suede inserts.
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| CN108330555A (en) * | 2018-02-10 | 2018-07-27 | 中科纺织研究院（青岛）有限公司 | A kind of stone needle polyester fiber and preparation method thereof |
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| CN113707871A (en) * | 2021-09-02 | 2021-11-26 | 和也健康科技有限公司 | Preparation of nanobelt lithium titanate @ stone needle composite fiber material, product and application |
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