CN107245879A - A kind of modified polyester fibre product, preparation method and its usage - Google Patents
A kind of modified polyester fibre product, preparation method and its usage Download PDFInfo
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- CN107245879A CN107245879A CN201710443947.3A CN201710443947A CN107245879A CN 107245879 A CN107245879 A CN 107245879A CN 201710443947 A CN201710443947 A CN 201710443947A CN 107245879 A CN107245879 A CN 107245879A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
Abstract
The present invention relates to a kind of modified polyester fibre product, the polyester fiber of the modified polyester fibre product is inside and outside to have graphene sheet layer；The terylene fiber products include polyester fiber, spun polyester thread and dacron.The present invention in the inside and outside attachment of polyester fiber or doses graphene simultaneously, adds the uniformity and fastness of graphene presence；The present invention improves the electric conductivity of polyester fiber by adding graphene and/or biomass graphene；Addition graphene oxide and/or biomass graphene further enhancing the far infrared performance of polyester fiber；The preparation method that the present invention is provided effectively can dose graphene to polyester fiber, while the coated graphite alkene lamella outside polyester fiber, graphene being uniformly distributed on polyester fiber is realized by terylene fiber products impregnated graphite alkene solution.
Description
Technical field
The invention belongs to fibre preparation field, and in particular to a kind of modified polyester fibre product, preparation method and its
Purposes, more particularly to a kind of conductive modified polyester fibre product, preparation method and its usage.
Background technology
The development of conductive fiber start from the 1960s, conductive fiber typically refer under standard environment (20 DEG C of temperature,
Humidity 65%), ratio resistance is less than 107Ω·cm.Its development course generally comprises 4 stages：Metallic fiber, carbon fiber and carbon containing
The composite conducting fiber of black composition polymer, the conductive fiber containing metal salt, conduction high polymer conductive fiber.Although conductive
Fiber has obtained significant progress, but there is also it is certain the problem of, such as by metallic conduction fiber and plate metal conductive fiber system
Into fabric feeling it is coarse, comfortableness is poor, and conducting polymer technique is more complicated, seriously polluted.Furthermore, pass through coating or letter
The compound firmness of fibre graphene prepared by single impregnation technology is not strong enough, and additional work(is just lost after washing repeatedly
Energy.Therefore, develop that the new new method for preparing conductive fiber is significant and actual application prospect.
Terylene is an important kind in synthetic fibers, is with p-phthalic acid (PTA) or terephthalic acid (TPA) diformazan
Ester (DMT) and ethylene glycol (EG) are raw material through esterification or fiber-forming polymer prepared by ester exchange and polycondensation reaction --- it is poly- to benzene
Naphthalate (PET), the fiber being made through spinning and post processing.
Graphene is a kind of two-dimensional material for the alveolate texture being made up of individual layer sp2 hydbridized carbon atoms, with many excellent
Different performance (high-strength, high heat conduction, highly conductive, high lightweight), while also possessing big pi-conjugated system.It has been found since 2004,
Graphene just becomes a big study hotspot of scientific circles.While the physicochemical properties to graphene are studied, with
The related composite of graphene emerges in an endless stream.Graphene is combined by prior art with textile fabric, it is desired to be able to had
While the functional fiber fiber such as electric conductivity and far infrared, the adhesion-tight degree of graphene is further ensured, makes its function
Do not decay significantly because of increasing for washing times.
This area needs to develop a kind of modified fibre product, itself and graphite alkenes Material cladding, can improve the fiber
The performances such as the electric conductivity or far infrared of product, while being ensured of the adhesion-tight degree of graphene.
The content of the invention
It is an object of the invention to provide a kind of modified polyester fibre product, the terylene of the modified polyester fibre product is fine
Dimension is inside and outside to have graphene sheet layer；
The terylene fiber products include polyester fiber, spun polyester thread and dacron.
The present invention passes through inside and outside while setting graphene sheet layer in polyester fiber, it is possible to increase graphene sheet layer exists
Fastness on polyester fiber, while improving branch uniformity of the graphene in polyester fiber radial direction.
Exemplarily, it is of the present invention to be spun comprising modified dacron yarn by the modified polyester fibre list, blending or with not
Modified polyester fibre blending is obtained.The fabric comprising modified polyester fibre is by the modified polyester fibre, and described include changes
The yarn of property polyester fiber is made.
Preferably, in modified polyester fibre of the present invention, it is present in the graphene film outside the modified polyester fibre
Layer is more than the graphene sheet layer being present in inside modified polyester fibre.There is more graphene outside the modified polyester fibre
Lamella, can overlap in the outside of modified polyester fibre, preferably improve the conduction of the modified polyester fibre product
Property.
Fiber has macromolecular material aggregation to obtain, and macromolecular is regular mutually neatly stable to be arranged in height
The geometrical regularity of degree, as crystalline texture or crystalline state.The region of the regular proper alignment of fiber macromolecular turns into crystallization
Area；In crystal region macromolecular chain segment arranged regular, close structure, gap and hole are less, and inter-molecular binding force is strong.Fiber divides greatly
The disorderly region arranged is noncrystalline domain to son at random, in noncrystalline domain, macromolecular chain segment fall into disarray, random, structure
Loosely, there are more gap and hole, the power that be combined with each other is small.
Preferably, the gross mass of graphene sheet layer is the total matter of modified polyester fibre product in the modified polyester fibre product
0.5~3wt% of amount.Graphene sheet layer content should not be excessive, is excessively easily caused fibre strength reduction, the wasting of resources.
In the present invention, include inside the modified polyester fibre crystal region, noncrystalline domain and the crystal region of fiber with
Gap between noncrystalline domain.
Gap of the present invention, space, hole can be replaced mutually, represent the space of fibrous inside.
Preferably, there is graphene sheet layer in the modified polyester fibre internal junction crystalline region, while the modified polyester fibre
There is graphene sheet layer in outside.
Preferably, particle diameter≤20 μm of the graphene sheet layer, such as 0.2 μm, 0.5 μm, 1 μm, 2 μm, 3 μm, 4 μm, 5 μ
M, 6 μm, 7 μm, 8 μm, 9 μm, 10 μm, 12 μm, 14 μm, 16 μm, 18 μm, 19 μm etc..
Preferably, the particle diameter of the graphene sheet layer existed inside the modified polyester fibre is less than 1 μm, such as 0.05 μm,
0.1 μm, 0.2 μm, 0.3 μm, 0.4 μm, 0.5 μm, 0.6 μm, 0.7 μm, 0.8 μm, 0.9 μm etc..
Preferably, the particle diameter of the graphene sheet layer existed outside the modified polyester fibre is 1~20 μm, such as 1 μm, 2 μ
M, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm, 10 μm, 12 μm, 14 μm, 16 μm, 18 μm, 19 μm etc..
Preferably, in the modified polyester fibre product polyester fiber ratio resistance≤1 × 105Ω cm, such as 1 × 104
Ω·cm、4×104Ω·cm、7×104Ω·cm、9×104Ω·cm、1×103Ω·cm、5×103Ω·cm、8×103
Ω·cm、1×102Ω cm, 1 × 10 Ω cm etc..
Preferably, when the graphene sheet layer is graphene oxide and/or biomass graphene, the modified dacron is fine
After fiber products are washed 50 times, its far infrared normal emittance is not less than 0.85, for example, be not less than 0.87, is not less than 0.88, no
Less than 0.90.
In order to further improve the intensity of the modified polyester fibre product and the fastness of graphene sheet layer, described changes
Contain nano-cellulose in property terylene fiber products.The addition of appropriate nano-cellulose can improve and wind graphene sheet layer
On the polyester fiber, and the winding of nano-cellulose can improve the intensity of the modified polyester fibre product.
Preferably, it is compounded with nano-cellulose in the modified fibre of the modified polyester fibre product.
Preferably, the nano-cellulose is wrapped in the modified polyester fibre internally and/or externally.Refer specifically to, receive
Rice cellulose is by high draw ratio and small diameter, by outside graphene sheet layer and fibrous inside crystal region or fibrous inside stone
Black alkene lamella is bundled or overlapped so that outside graphene sheet layer is difficult for drop-off.
The two of the object of the invention are to provide a kind of preparation method of the modified fibre product as described in the first purpose, the side
Method includes impregnating unmodified terylene fiber products in graphene sheet layer dispersion liquid, afterwards through supercooling, drying, obtains everywhere
Terylene fiber products after reason；Wherein, the temperature of the dipping is the glass transition temperature more than terylene and the glutinous stream less than terylene
Temperature, preferably 85~120 DEG C.
Unmodified terylene fiber products are immersed in the glass transition temperature more than terylene and the glutinous stream temperature less than terylene,
For example in 80~120 DEG C of dispersion liquid, the dipping temperature of the dispersion liquid is in the glass transition temperature and elastomeric state of polyester fiber
Between temperature, the glass transition temperature can improve the motion of macromolecular in the fiber so that crystal region is to noncrystalline
Area is converted so that the space of noncrystalline domain becomes big so that the space between crystal region and noncrystalline domain between the macromolecular in region becomes
Greatly；The particle for the graphene sheet layer being dispersed in simultaneously in graphene sheet layer dispersion liquid enters described space；It is then impregnated
Fiber is cooled down so that the graphene in dipping process into the space is fixed on fibrous inside, and because the larger quilt of particle diameter
Keep off graphene sheet layer outside space can to coat, laminating, or even can be partly to enter fibrous inside, partly outside fiber
The form in portion is present.
Those skilled in the art are it will be clearly understood that fibrous inside of the present invention and fibrous external are well known in the art general
Read, it is understood that the macromolecular into fiber is in space clustering formation supramolecular structure, the inside of the macromolecular aggregation in groups
There is the region between crystal region, noncrystalline domain and crystal region and noncrystalline domain；And macromolecular aggregation finishes the outside to be formed and seen
Do the outside of fiber.
Preferably, the modified polyester fibre product include modified polyester fibre, the yarn comprising modified polyester fibre and
Any a kind or at least two kinds of of combination in fabric comprising modified polyester fibre.Furtherly, terylene fiber products can be
Polyester fiber, can be spun polyester thread or polyester fabric；Can be polyester fiber impregnated graphite alkene solution, can be with
It is spun polyester thread impregnated graphite alkene solution, can is polyester fabric impregnated graphite alkene solution.
Preferably, the graphene sheet layer include graphene, graphene oxide, any a kind of Graphene derivative or extremely
Few 2 kinds mixing.
Preferably, graphene is prepared including graphite by stripping method, and graphene oxide is prepared by reduction, stone
Ink is prepared by redox, and carbonaceous gas is prepared by CVD, and high-temperature cracking method is passed through by raw material of biomass
Prepare.
Preferably, the graphene oxide includes the graphene that TEMPO systems are aoxidized.
The graphene of TEMPO systems oxidation can insert oxidisability functional group inside graphene, improve graphene oxide
Dispersing uniformity in dispersion liquid, reduces the reunion of graphene in graphene dispersing solution, improves the utilization rate of graphene.
Preferably, the Graphene derivative includes any 1 in element doping graphene or functional group's graphite alkene thing
Plant or at least two kinds of combinations.
Preferably, the concentration of the graphene sheet layer dispersion liquid be 0.1~5wt%, preferably 0.3~2wt%, for example
0.3%th, 0.5%, 0.8%, 0.9%, 1.3%, 1.6%, 1.8%, 1.9%, 1.5%, 3%, 3.6%, 4%, 4.5% etc..
Preferably, the particle diameter of the graphene sheet layer in the graphene sheet layer dispersion liquid is no more than 20 μm, is preferably
100nm~10 μm, further preferred 200nm~5 μm；Such as 30nm, 150nm, 190nm, 230nm, 260nm, 290nm,
330nm, 460nm, 590nm, 630nm, 760nm, 890nm, 930nm, 1 μm, 3 μm, 8 μm, 11 μm, 13 μm, 18 μm etc..
Preferably, the dip time be 15~120min, such as 16min, 19min, 23min, 26min, 32min,
55min, 66min, 73min, 78min, 85min, 88min, 95min etc..
Graphene oxide electric conductivity itself is poor, in order to ensure the conduction for the fibre being modified by graphene oxide
Property, the present invention can carry out reduction treatment to the modified fibre product for being compounded with graphene oxide.
Preferably, when the graphene sheet layer includes graphene oxide, also original place is carried out before cooling and/or afterwards
Reason.
Preferably, the method for the reduction treatment includes reducing agent reducing process and/or heating reducing process.
Preferably, the reducing agent reducing process is reduced including adding reducing agent.
Preferably, the addition of the reducing agent is the 10~200wt%, preferably 50~100wt% of graphene sheet layer.
Preferably, the reducing agent includes ascorbic acid, hydrazine hydrate, glucose, ethylenediamine, sodium citrate, the Guang ammonia of L- half
Any a kind or at least two kinds of of combination in acid, hydroiodic acid or sodium borohydride.
Preferably, the heating reducing process is included in non-oxidizing atmosphere, and heating is reduced.
Preferably, the heating reducing process step includes：In autoclave, protective atmosphere and/or reduction are passed through
Property atmosphere, heating reduction；Temperature≤200 DEG C of the heating reduction, pressure≤1.6MPa.
Preferably, nano-cellulose is added with the graphene sheet layer dispersion liquid.
Preferably, the diameter of the nano-cellulose is not more than 10nm, and draw ratio is not less than 10, and draw ratio can be 20,
30,50,100 etc..
Preferably, concentration of the nano-cellulose in dispersion liquid be below 2wt%, preferably below 1wt%, further preferably
Below 0.5wt%.
Nano-cellulose is in itself wire, and it fibrous external can circumferentially be wound again, and this canoe can be improved
The intensity of fiber, and firmness of the graphene in fibrous external can be improved；On the other hand, one end of nano-cellulose can
Insert in graphene sheet layer, improve adhesion amount of the graphene sheet layer on fiber.But nano-cellulose is non-conductive in itself, excessively
Nano-cellulose can cause the decline of electric conductivity.
As optional technical scheme, described impregnate unmodified terylene fiber products in graphene sheet layer dispersion liquid is divided
Two steps are carried out, and specifically include following steps：
(A1) unmodified terylene fiber products are impregnated into the first graphene sheet layer dispersion liquid, obtains the first dipping and wash
Synthetic fibre fibre；The particle diameter of graphene sheet layer is less than 1 μm in the first graphene sheet layer dispersion liquid；
(A2) the first dipping terylene fiber products are impregnated into the second graphene sheet layer dispersion liquid, obtains the second dipping and wash
Synthetic fibre fibre；The particle diameter of graphene sheet layer is 1~20 μm in the second graphene sheet layer dispersion liquid.
The step (A1) and (A2) dipping temperature are the glass transition temperature more than terylene and the glutinous stream temperature less than terylene,
It is preferred that 80~120 DEG C, and the step (A2) dipping temperature is less than step (A1) dipping temperature.
Because the size of polyester fiber internal voids is limited, step (A1) is less than 1 μm of graphene sheet layer only with particle diameter
Terylene fiber products are modified, it is well known that graphene particle diameter is smaller to be less susceptible to disperse, it is easier to reunite therefore past
Toward the graphene solution of selection low concentration, the consumption of graphene is so also saved, and reduces big particle diameter graphene sheet layer and is blocked up
The probability in space is filled in, the adhesion amount of graphene is improved.It is 1~20 μm of graphene sheet layer to terylene that step (A2), which uses particle diameter,
Fibre is modified, and big particle diameter graphene sheet layer can be made to be present in fibrous external in the way of coating, fit, more favorably
Conductive network is formed outside polyester fiber in graphene, additionally it is possible to play a part of closing fibrous inside space, by increasing capacitance it is possible to increase
Fastness of the graphene sheet layer in polyester fiber.
The three of the object of the invention are to provide a kind of purposes of the modified polyester fibre product as described in the first purpose, the modification
Terylene fiber products are used to prepare home textile, underwear, protective garment, thermal cloth, socks.
Compared with prior art, the present invention has the advantages that：
(1) present invention in the inside and outside attachment of polyester fiber or doses graphene simultaneously, adds graphene presence
Uniformity and fastness；
(2) present invention improves the electric conductivity of polyester fiber by adding graphene and/or biomass graphene；Addition
Graphene oxide and/or biomass graphene further enhancing the far infrared performance of polyester fiber；
(3) preparation method that the present invention is provided effectively can dose graphene to polyester fiber, while washing
Synthetic fibre fibrous external coated graphite alkene lamella, realizes graphene on polyester fiber by terylene fiber products impregnated graphite alkene solution
Be uniformly distributed.
Embodiment
Technical scheme is further illustrated below by embodiment.
Those skilled in the art it will be clearly understood that the embodiment be only to aid in understand the present invention, be not construed as to this hair
Bright concrete restriction.
Embodiment 1~7
A kind of modified polyester fibre, specific steps include：
(1) particle diameter for preparing graphene in the first graphene dispersing solution, first graphene dispersing solution is less than 1 μm；Match somebody with somebody
The particle diameter of graphene in the second graphene dispersing solution, second graphene dispersing solution is made between 1~2 μm；
(2) polyester fiber is impregnated into the first graphene dispersing solution in the first temperature, takes out be impregnated with the first graphene afterwards
Polyester fiber, and continued to be immersed in the second graphene dispersing solution and impregnate 30min, taken out afterwards, dry, be modified
Polyester fiber.
Performance test：By obtained modified polyester fibre according to GB/T 14342-2015 to obtained modified polyester fibre
Detected；Modified polyester fibre is washed 50 times afterwards, continued according to GB/T 14342-2015 to the modified dacron after washing
Fiber is detected.
Process conditions and the test result of obtained modified polyester fibre that table 1 gives embodiment 1~7.
Table 1：Embodiment 1~7 prepares the process conditions and test result of modified polyester fibre
It can be seen from Table 1 that, when the dipping temperature of embodiment 6 first is less than the second dipping temperature, due to double-steeping
When fiber polymer motion ratio impregnate violent for the first time, cause the graphene for being immersed in fibrous inside for the first time to overflow, hinder simultaneously
Hinder second of dipping effect so that ratio resistance is raised；When graphene particle diameter is more than the second maceration extract in the maceration extract of embodiment 7 first
Graphene particle diameter when so that fibrous inside graphene content is relatively low, and outside content is higher, it is inside and outside between do not form stronger
Active force, cause washing times increase graphene come off it is more obvious.
Embodiment 8~11
A kind of modified polyester fibre, the difference with embodiment 3 is, same in step (2) first graphene dispersing solution
When scattered nano-cellulose (draw ratio 80~120, below diameter 10nm), concentration of the nano-cellulose in dispersion liquid is
0.1wt% (embodiment 8), 0.5wt% (embodiment 9), 1wt% (embodiment 10), 2wt% (embodiment 11).
Using performance test methods same as Example 3, test result is shown in Table 2.
Embodiment 12
A kind of modified polyester fibre, the difference with embodiment 3 is, the first and second graphene dispersing solutions are all replaced with
Graphene oxide dispersion, and reduction step is carried out, it is specially：In step 2) take out the polyester fiber that dipping has impregnated for the second time
After be put into hydrazine hydrate reduction liquid carry out reduction treatment after, dry, obtain modified polyester fibre.Using same as Example 3
Performance test methods, test result is shown in Table 2.
Embodiment 13
A kind of modified polyester fibre, the difference with embodiment 3 is, the first and second graphene dispersing solutions are all replaced
For biomass graphene dispersing solution.
Using performance test methods same as Example 3, test result is shown in Table 2.
In addition, the far infrared normal emittance (method of testing FZ/T64010-2000) of the present embodiment modified polyester fibre reaches
To 0.9.
Embodiment 14
A kind of modified polyester fibre, specific steps include：
(1) particle diameter of graphene in graphene dispersing solution, the graphene dispersing solution is prepared between 0.1~3 μm；
(2) polyester fiber is taken out afterwards in 95 DEG C of impregnated graphite alkene dispersion liquid 30min, dried, obtain modified dacron fine
Dimension.
Using performance test methods same as Example 3, test result is shown in Table 2.
Embodiment 15-16
Fiber in embodiment 3 is replaced with into the yarn (embodiment 15) that match network compact spinning is spun into, and knitting fabric (is implemented
Example 16).
Table 2 gives the test result for the modified polyester fibre product that embodiment 8~16 is obtained.
Table 2：The test result of the modified polyester fibre product of embodiment 8~16
| Embodiment | Do not wash ratio resistance, Ω cm | Ratio resistance after washing 50 times, Ω cm |
| Embodiment 8 | 1×102 | 1×102 |
| Embodiment 9 | 1×102 | 1×102 |
| Embodiment 10 | 1×102 | 2×102 |
| Embodiment 11 | 8×103 | 9×103 |
| Embodiment 12 | 3×102 | 8×102 |
| Embodiment 13 | 2×102 | 5×102 |
| Embodiment 14 | 6×104 | 1×105 |
| Embodiment 15 | 3×102 | 6×102 |
| Embodiment 16 | 2×102 | 6×102 |
In table 2, the yarn of embodiment 15 can be knitted into fabric, detection sheet resistance is carried out using GB12703.4-2010
Rate, the surface resistivity do not washed is 2 × 102Ω, the surface resistivity that washing is 50 times is 7 × 102Ω；The fabric of embodiment 16
Surface resistivity is detected that the surface resistivity do not washed is 2 × 10 using GB12703.4-20102Ω, is washed 50 times
Surface resistivity is 6 × 102Ω。
Comparative example 1
A kind of modified polyester fibre, is modified to polyester fiber body by the way of In-situ reaction, concretely comprised the following steps：
(1) 200g graphenes and 8.52kgPTA, 3.5L ethylene glycol are fed intake mixing, are introduced directly into after ball-milling treatment 20min
To mashing kettle mashing 30min, reacted according to using three kettle PET polymerization techniques, carry out polymerisation, polymerisation is finished
To melt；
(2) melt is in 40 DEG C of cooling waters, and 0.5m/s draft speed condition bottom discharges, directly granulation obtain graphene and be combined
PET master batch；
(3) graphene is combined PET master batch at 110 DEG C, after drum dried 24h, is directly used in melt spinning, spinning goes out
Silk is cooled down using water smoke, 40 DEG C of chilling temperature, 35 DEG C of drying temperature, and melt spinning obtains modified polyester fibre.
Obtained fiber is detected according to GB/T 14342-2015, its ratio resistance do not washed is 1 × 1013Ω·
cm。
Comparative example 2
A kind of modified polyester fibre, is modified by the way of normal temperature dipping, is concretely comprised the following steps：
(1) particle diameter of graphene in graphene dispersing solution, the graphene dispersing solution is prepared between 0.1~3 μm；
(2) polyester fiber is taken out afterwards in 25 DEG C of impregnated graphite alkene dispersion liquid 30min, dries, obtain modified fibre.
Obtained fiber is detected according to GB/T 14342-2015, its ratio resistance do not washed is 1 × 104Ω·
Cm, the ratio resistance after washing 20 times is 1 × 1010Ω·cm。
Applicant states that the present invention illustrates the process of the present invention, but not office of the invention by above-described embodiment
It is limited to above-mentioned processing step, that is, does not mean that the present invention has to rely on above-mentioned processing step and could implemented.Art
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to raw material selected by the present invention
Addition, selection of concrete mode etc., within the scope of all falling within protection scope of the present invention and being open.
Claims (9)
1. a kind of modified polyester fibre product, it is characterised in that inside the polyester fiber of the modified polyester fibre product and outer
There is graphene sheet layer in portion；
The terylene fiber products include polyester fiber, spun polyester thread or dacron.
2. modified polyester fibre product as claimed in claim 1, it is characterised in that be present in outside the modified polyester fibre
Graphene sheet layer be more than and be present in graphene sheet layer inside modified polyester fibre；
Preferably, the gross mass of graphene sheet layer is modified polyester fibre product gross mass in the modified polyester fibre product
0.5~3wt%；
Preferably, crystal region, noncrystalline domain and crystal region and the noncrystalline domain of fiber are included inside the modified polyester fibre
Between gap；
Preferably, there is graphene sheet layer in the modified polyester fibre internal junction crystalline region, while outside the modified polyester fibre
There is graphene sheet layer；
Preferably, particle diameter≤20 μm of the graphene sheet layer；
Preferably, the particle diameter of the graphene sheet layer existed inside the modified polyester fibre is less than 1 μm；
Preferably, the particle diameter of the graphene sheet layer existed outside the modified polyester fibre is 1~20 μm.
3. modified fibre product as claimed in claim 1 or 2, it is characterised in that terylene in the modified polyester fibre product
Ratio resistance≤1 × 10 of fiber5Ω·cm；
Preferably, after the modified polyester fibre product is washed 50 times, ratio resistance≤1 × 10 of polyester fiber5Ω·cm。
4. the modified polyester fibre product as described in one of claims 1 to 3, it is characterised in that the modified fibre product
Nano-cellulose is compounded with fiber；
Preferably, the nano-cellulose is wrapped in the fiber internally and/or externally.
5. the preparation method of a kind of modified polyester fibre product as described in one of Claims 1 to 4, it is characterised in that described
Method includes impregnating unmodified terylene fiber products in graphene sheet layer dispersion liquid, afterwards through supercooling, drying, obtains
Fibre after processing；
Wherein, the temperature of the dipping is the glass transition temperature more than terylene and the glutinous stream temperature less than terylene；
Preferably, the temperature of the dipping is 80~120 DEG C.
6. preparation method as claimed in claim 5, it is characterised in that the graphene sheet layer includes graphene, graphite oxide
Any a kind or at least two kinds of of mixing of alkene, Graphene derivative；
Preferably, graphene is prepared including graphite by stripping method, graphene oxide is prepared by reduction, graphite leads to
Oxidization-reduction is prepared, carbonaceous gas is prepared by CVD, prepared by raw material of biomass by high-temperature cracking method
Any a kind or at least two kinds of of combination in obtaining；
Preferably, the concentration of the graphene sheet layer dispersion liquid is 0.1~5wt%, preferably 0.3~2wt%；
Preferably, the particle diameter of the graphene sheet layer in the graphene sheet layer dispersion liquid is no more than 20 μm；Preferably 100nm~
10 μm, further preferred 200nm~5 μm；
Preferably, the dip time is 15~120min；
Preferably, when the graphene sheet layer includes graphene oxide, reduction treatment is carried out before cooling and/or afterwards；
Preferably, the method for the reduction treatment includes reducing agent reducing process and/or heating reducing process；
Preferably, the reducing agent reducing process is reduced including adding reducing agent；
Preferably, the addition of the reducing agent is the 10~200wt%, preferably 50~100wt% of graphene sheet layer；
Preferably, the reducing agent includes ascorbic acid, hydrazine hydrate, glucose, ethylenediamine, sodium citrate, Cys, hydrogen
Any a kind or at least two kinds of of combination in acid iodide or sodium borohydride；
Preferably, the heating reducing process is included in non-oxidizing atmosphere, and heating is reduced；
Preferably, the heating reducing process step includes：In autoclave, protective atmosphere and/or reproducibility gas are passed through
Atmosphere, heating reduction；Temperature≤200 DEG C of the heating reduction, pressure≤1.6MPa.
7. the preparation method as described in claim 5 or 6, it is characterised in that be added with and receive in the graphene sheet layer dispersion liquid
Rice cellulose；
Preferably, the diameter of the nano-cellulose is not more than 10nm, and draw ratio is not less than 10；
Preferably, concentration of the nano-cellulose in dispersion liquid be below 2wt%, preferably below 1wt%, further preferably
Below 0.5wt%.
8. the preparation method as described in one of claim 5~7, it is characterised in that by the unmodified terylene fiber products
Impregnate and be carried out in two steps in graphene sheet layer dispersion liquid, specifically include following steps：
(A1) unmodified terylene fiber products are impregnated into the first graphene sheet layer dispersion liquid, obtains the first dipping polyester fiber
Product；The particle diameter of graphene sheet layer is less than 1 μm in the first graphene sheet layer dispersion liquid；
(A2) the first dipping terylene fiber products are impregnated into the second graphene sheet layer dispersion liquid, obtains the second dipping terylene fine
Fiber products；The particle diameter of graphene sheet layer is 1~20 μm in the second graphene sheet layer dispersion liquid；
Preferably, the step (A1) and (A2) dipping temperature are the glass transition temperature more than terylene and the glutinous stream temperature less than terylene
Degree, preferably 80~120 DEG C, and the step (A2) dipping temperature is less than step (A1) dipping temperature.
9. a kind of purposes of the modified polyester fibre product as described in one of Claims 1 to 4, it is characterised in that the Modified Polyester
Synthetic fibre fibre is used to prepare home textile, underwear, protective garment, thermal cloth, socks.
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710443947.3A CN107245879A (en) | 2017-06-13 | 2017-06-13 | A kind of modified polyester fibre product, preparation method and its usage |
| PCT/CN2018/079035 WO2018166477A1 (en) | 2017-03-15 | 2018-03-14 | Modified fibre product, preparation method therefor and use thereof |
| JP2019572277A JP6852200B2 (en) | 2017-03-15 | 2018-03-14 | Modified textile products, preparation methods and their use |
| KR1020197030234A KR20190125480A (en) | 2017-03-15 | 2018-03-14 | Modified textile products, manufacturing methods and uses thereof |
| DE112018001356.1T DE112018001356T5 (en) | 2017-03-15 | 2018-03-14 | Modified fiber product, manufacturing method thereof and use thereof |
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| CN109137478A (en) * | 2018-07-02 | 2019-01-04 | 张家港锦亿化纤有限公司 | A kind of production method of conductive dacron fibre |
| CN109914099A (en) * | 2019-04-10 | 2019-06-21 | 宁波博洋家纺集团有限公司 | A kind of preparation process of hydrophilic resistant textile fabric |
| CN112900076A (en) * | 2021-01-31 | 2021-06-04 | 福建沃凯丝化纤有限公司 | Multifunctional polyester fiber and preparation method thereof |
| CN113680138A (en) * | 2020-05-19 | 2021-11-23 | 济南圣泉集团股份有限公司 | Antistatic filter material and preparation method and application thereof |
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