CN108929446A - Graphene composite master batch, modified fibre, superfiber leather and preparation method thereof purposes - Google Patents
Graphene composite master batch, modified fibre, superfiber leather and preparation method thereof purposes Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
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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
- D01F1/103—Agents inhibiting growth of microorganisms
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0004—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using ultra-fine two-component fibres, e.g. island/sea, or ultra-fine one component fibres (< 1 denier)
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0011—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using non-woven fabrics
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/125—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyamides
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
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Abstract
Graphene composite master batch, modified fibre, superfiber leather and preparation method thereof purposes.The present invention relates to a kind of preparation method of graphene composite master batch, the preparation method includes the following steps：(1) substrate is divided into n parts, and the quality of (n+1)th part of substrate is less than 10 times of n-th part of substrate mass；(2) the 1st part of substrate is mixed with grapheme material, obtains the 1st masterbatch mix；(3) (n+1)th part of substrate is mixed with n-th masterbatch mix, obtains (n+1)th masterbatch mix, as graphene composite master batch；Wherein n takes positive integer.The present invention obtains the evenly dispersed master batch for having grapheme material, reduces graphene agglomeration by adjusting the hybrid mode of graphene and substrate, improves the antibiotic property and far infrared performance of master batch.
Description
Technical field
The invention belongs to synthetic leather fields, and in particular to a kind of graphene composite master batch and preparation method thereof, using described
The modified fibre and preparation method thereof that graphene composite master batch is prepared, the ultra-fine fibre being prepared using the modified fibre
Dimension leather and preparation method thereof purposes.
Background technique
Since the resource of natural leather is limited, with the progress of science and technology and the raising of living standards of the people, open
Hair develops the emulational leather of high-quality to meet the needs of market, becomes urgent problem.Artificial tanning's industrialization production
Existing decades history, with the continuous application of various new materials, product is also being constantly updated.Superfine fiber chemical leather (letter
Claim " super fiber leather ") it has been rapidly developed as the artificial synthesized leather of the third generation.The primary raw material of super fiber leather manufacture is that pencil is super
Fine fibre and polyurethane.Super fiber leather product is checked through various aspects and practice, and tearing strength and tensile strength are high, and folding resistance is good, imitates
True property is good, surface easy cleaning.But there is also certain defects for the biocidal property of this super fiber leather and antibiotic property, especially as system
The raw material for making the expensive goods such as leather shoes, fur clothing, sofa, automobile interior decoration, using over time, leather surface just will appear mildew, tortoise
Phenomenon is split, so that not being available and losing value.It would therefore be desirable to have a kind of super fiber leathers for being able to suppress pernicious bacteria to facilitate people
Life.
Current main bacteriostatic agent has inorganic metal compound such as zeolite with carrying silver, carries silver-colored silicate, organo-metallic compound
Such as quaternary ammonium salt, pyridines, imidazoles, natural organic matter such as chitosan.The method that bacteriostatic agent loads on leather is mainly had
Two kinds：Direct addition method and finishing method.But this antibacterial measure have the defects that it is certain because bacteriostatic agent is to add
, rather than possessed by substance itself, so the long-time with product uses, antibacterial substance can gradually fall off, cause to produce
Product lose bacteria resistance function.Meanwhile because certain pollution can be also caused to environment using some heavy metal ion.
A kind of synthetic leather with anti-microbial property how is obtained, or is ability for the fibrous material or master batch of synthetic leather
The domain technical issues that need to address.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of graphene composite master batch, the preparation method includes as follows
Step：
(1) substrate is divided into n parts, and the quality of (n+1)th part of substrate is less than 10 times of n-th part of substrate mass；
(2) the 1st part of substrate is mixed with grapheme material, obtains the 1st masterbatch mix；
(3) (n+1)th part of substrate is mixed with n-th masterbatch mix, obtains (n+1)th masterbatch mix, as graphene is multiple
Close master batch；
Wherein n takes positive integer, such as 1,2,3,4,5 etc..
Substrate is divided into n parts by the present invention, is successively mixed with grapheme material, and the quality for limiting (n+1)th part of substrate is less than
10 times of n-th part of substrate mass, can be realized the evenly dispersed of grapheme material, reduce the reunion of graphene, to the greatest extent
Play the value of graphene.
As one of optimal technical scheme, the preparation method includes the following steps：
(1) substrate is divided into 2 parts, and the quality of the 2nd part of substrate is less than 10 times of the 1st part of substrate mass；
(2) the 1st part of substrate is mixed with grapheme material, obtains the 1st masterbatch mix；
(3) the 2nd part of substrate is mixed with the 1st masterbatch mix, obtains the 2nd masterbatch mix, the as compound mother of graphene
Grain.
The present invention limits 10 times of the quality of the 2nd part of substrate less than the 1st part of substrate mass by the way that substrate is divided into 2 parts,
Substrate can be thus achieved to mix with the uniform of grapheme material.
Preferably, the mass ratio of step (2) grapheme material and the 1st part of substrate is 1:10~100, such as 1:20,
1:30,1:40,1:50,1:60,1:70,1:80,1:90 etc..
Preferably, step (2) mode for mixing the 1st part of substrate with grapheme material includes the following steps：
(2a) mixes the 1st part of substrate with the grapheme material of partial size D90≤1 μm；
(2b) mixes the mixed material of step (2a) with the grapheme material of 1 μm of D90≤8 μm < of partial size.
The grapheme material of partial size D90≤1 μm is first mixed with the 1st part of substrate, later with 1 μm of D90≤8 μm < of partial size
Grapheme material mixing, enables to being more evenly distributed for the graphene of different-grain diameter, i.e., is distributed not in identical range
It is identical with the quantity of the graphene of partial size.
Preferably, the grapheme material of partial size D90≤1 μm and the grapheme material of 1 μm of D90≤8 μm < of partial size
Mass ratio is 1:1~5, such as 1:2,1:3,1:4 etc..
Preferably, in terms of by the gross mass of graphene composite master batch for 100 parts by weight, the quality of the grapheme material is 5
~10 parts by weight, such as 6 parts by weight, 7 parts by weight, 8 parts by weight, 9 parts by weight etc..
Preferably, the grapheme material includes graphene, any a kind or at least two kinds of of group in Graphene derivative
Close, preferably redox graphene, graphene oxide, biomass material preparation graphene, removing graphite obtain graphene,
Any a kind or at least two kinds of of the combination being vapor-deposited in obtained graphene.
Preferably, the substrate includes polypropylene fibre master batch, dacron master grain, chinlon master batch, spandex master batch, appointing in acrylic fibers master batch
The combination of a kind or at least two kinds of of meaning.
The second object of the present invention is to providing a kind of graphene composite master batch, the graphene composite master batch passes through the second purpose
The preparation method is prepared.
The three of the object of the invention are to provide a kind of preparation method of modified fibre, and the preparation method includes：
Graphene composite master batch described in the second purpose and blank slice are mixed to get mixture, carry out spinning later.
Preferably, the component of the mixture includes following component in parts by weight：
5~15 parts of graphene composite master batch
Blank is sliced 85~95 parts
The sum of described mixture each component is 100 parts by weight.
Preferably, the partial size of graphene composite master batch described in the second purpose is less than or equal to the partial size of blank slice,
It is preferred that the ratio between graphene composite master batch described in the second purpose and the partial size of blank slice are 1:2~10, such as 1:3,1:4,1:
5,1:6,1:7,1:8,1:9 etc..
The four of the object of the invention are to provide a kind of preparation method for determining island sea-island composite fiber, and the preparation method includes
Following steps：
Graphene composite master batch described in the second purpose is added in the component of island, obtains being mixed with graphene composite master batch
Island component, then by sea component be mixed with the island component of graphene composite master batch melting mixing during melt spinning,
Spinning is carried out later, obtains island fiber with figured sea-island.
Preferably, the island component for being mixed with graphene composite master batch includes following component in parts by weight：
5~15 parts of graphene composite master batch
85~95 parts of island component
The sum of described mixture each component is 100 parts by weight；
Preferably, the partial size of graphene composite master batch described in the second purpose is less than or equal to the partial size of island component, excellent
Selecting the ratio between partial size of graphene composite master batch described in the second purpose and island component is 1:2~10, such as 1:3,1:4,1:5,1:
6,1:7,1:8,1:9 etc..
Preferably, the sea component be mixed with graphene composite master batch island component mixed proportion be 30%~
40%:70%~60%, such as 31%:69%, 32%:68%, 33%:67%, 34%:66%, 35%:65%, 36%:
64%, 37%:63%, 38%:62%, 39%:61% etc..
Preferably, 37 island island Shuo Wei for determining island sea-island composite fiber.
Optionally, it after " spinning " step, is oiled, drawing-off, drying steps.
The five of the object of the invention be to provide it is a kind of determine island sea-island composite fiber, it is described to determine island sea-island composite fiber and pass through
Preparation method described in the fourth purpose is prepared.
The object of the invention sixth is that provide a kind of preparation method of superfiber leather, the preparation method includes following step
Suddenly：
(I) determined island sea-island composite fiber with as claimed in claim 7 and prepared non-woven fabrics；
(II) by the non-woven fabrics impregnating polyurethane solution of step (I)；
(III) non-woven fabrics after step (II) to be impregnated to polyamide solution coagulates in dimethylformamide in water
Gu after washing, removing the sea component determined in the sea-island composite fiber of island by Alkali reduction；
(IV) step (III) treated non-woven fabrics is dry, obtain superfiber leather；
Preferably, the concentration of step (III) described dimethylformamide in water be 20~50wt%, such as 22wt%,
25wt%, 27wt%, 28wt%, 32wt%, 35wt%, 37wt%, 38wt%, 42wt%, 45wt%, 47wt%, 48wt%
Deng.
Preferably, the temperature of the solidification is 20~50 DEG C, such as 22 DEG C, 25 DEG C, 27 DEG C, 32 DEG C, 35 DEG C, 38 DEG C, 42
DEG C, 48 DEG C etc., the time is 30~60min, such as 35min, 40min, 45min, 55min, 60min etc..
Preferably, the temperature of the washing is 40~70 DEG C, such as 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C etc..
Preferably, the Alkali reduction, which removes, determines the mode of the sea component in the sea-island composite fiber of island and is：
Non-woven fabrics after washing is immersed in the NaOH solution that concentration is 15~30g/L, temperature is 80~100 DEG C, is located
Manage 30~60min of substrate.
The object of the invention seventh is that provide a kind of superfiber leather, the superfiber leather passes through system described in the sixth purpose
Preparation Method is prepared.
The object of the invention eighth is that providing a kind of purposes of superfiber leather, the superfiber leather is used to prepare shoes, case
Packet, furniture or automobile interior decoration.
Compared with prior art, the invention has the advantages that：
(1) for the present invention by adjusting the hybrid mode of graphene and substrate, obtaining evenly dispersed has grapheme material
Master batch reduces graphene agglomeration, improves the antibiotic property and far infrared performance of master batch；
(2) further, the present invention obtains different-grain diameter stone by the way that substrate is added portionwise in the graphene of different-grain diameter
Black alkene material is uniformly distributed, and further improves being uniformly distributed for master batch inside grapheme material；
(3) present invention prepares superfine fibre by being mixed with the substrate of grapheme material, assigns superfine fibre excellent suppression
Bacterium performance, after the superfine fibre and polyurethane are prepared synthetic leather, can slow down for a long time using mildew occurs, cracking shows
As.
Specific embodiment
The technical scheme of the invention is further explained by means of specific implementation.
Those skilled in the art are not construed as to this hair it will be clearly understood that the described embodiments are merely helpful in understanding the present invention
Bright concrete restriction.
The grapheme material of Examples 1 to 8 and comparative example 1 is the graphene being prepared using biomass as raw material, preparation
Method can refer to the method that patent publication No. is 104016341 embodiment 1 of CN, and substrate is chinlon master batch.
Embodiment 1
A kind of preparation method of graphene composite master batch, includes the following steps：
(1) substrate is divided into 2 parts, first part of substrate 1kg, second part of substrate 5kg；
(2) the 1st part of substrate is mixed with 100g grapheme material, obtains the 1st masterbatch mix；
(3) the 2nd part of substrate is mixed with the 1st masterbatch mix, obtains the 2nd masterbatch mix, the as compound mother of graphene
Grain.
Embodiment 2
A kind of preparation method of graphene composite master batch, includes the following steps：
(1) substrate is divided into 2 parts, first part of substrate 1kg, second part of substrate 5kg；
(2a) mixes the 1st part of substrate with the 30g partial size D90 grapheme material for being 1 μm；
(2b) mixes the mixed material of step (2a) with the 70g partial size D90 grapheme material for being 8 μm；
(3) the 2nd part of substrate is mixed with the 1st masterbatch mix, obtains the 2nd masterbatch mix, the as compound mother of graphene
Grain.
Embodiment 3
A kind of preparation method of graphene composite master batch, includes the following steps：
(1) substrate is divided into 2 parts, first part of substrate 1kg, second part of substrate 5kg；
(2a) mixes the 1st part of substrate with the 17g partial size D90 grapheme material for being 0.5 μm；
(2b) mixes the mixed material of step (2a) with the 83g partial size D90 grapheme material for being 5 μm；
(3) the 2nd part of substrate is mixed with the 1st masterbatch mix, obtains the 2nd masterbatch mix, the as compound mother of graphene
Grain.
Embodiment 4
A kind of preparation method of graphene composite master batch, includes the following steps：
(1) substrate is divided into 2 parts, first part of substrate 1kg, second part of substrate 5kg；
(2a) mixes the 1st part of substrate with the 50g partial size D90 grapheme material for being 0.1 μm；
(2b) mixes the mixed material of step (2a) with the 50g partial size D90 grapheme material for being 3 μm；
(3) the 2nd part of substrate is mixed with the 1st masterbatch mix, obtains the 2nd masterbatch mix, the as compound mother of graphene
Grain.
Embodiment 5
A kind of preparation method of graphene composite master batch, includes the following steps：
(1) substrate is divided into 2 parts, first part of substrate 1kg, second part of substrate 5kg；
(2a) mixes the 1st part of substrate with the 50g partial size D90 grapheme material for being 0.3 μm；
(2b) mixes the mixed material of step (2a) with the 100g partial size D90 grapheme material for being 8 μm；
(3) the 2nd part of substrate is mixed with the 1st masterbatch mix, obtains the 2nd masterbatch mix, the as compound mother of graphene
Grain.
Embodiment 6
A kind of preparation method of graphene composite master batch, the difference from embodiment 1 is that step (2) grapheme material adds
Dosage is 50g.
Embodiment 7
A kind of preparation method of graphene composite master batch, the difference from embodiment 1 is that step (2) grapheme material adds
Dosage is 80g.
Embodiment 8
A kind of preparation method of graphene composite master batch, the difference from embodiment 1 is that (1) first part of substrate 1kg of step,
Second part of substrate 8kg.
Comparative example 1
A kind of preparation method of graphene composite master batch, the difference from embodiment 1 is that (1) first part of substrate 1kg of step,
Second part of substrate 12kg.
Embodiment 9
A kind of preparation method of graphene composite master batch, the difference from embodiment 1 is that, substrate is dacron master grain.
Embodiment 10
A kind of preparation method of graphene composite master batch, the difference from embodiment 1 is that, the grapheme material is oxidation
Graphene, substrate are dacron master grain.
Application examples
A kind of superfine fibre, preparation method include the following steps：
(1) chip drying：
Sea, island component are subjected to chip drying respectively, are 30~50ppm for island component requirements moisture content, for extra large group
The requirement moisture content divided is 30~100ppm；
(2) melting and spinning：
Dried sea, island component slices are passed through feeding system respectively to put into respective spinning storage tank, simultaneously
The graphene composite master batch of Examples 1 to 10 and comparative example 1 is added in the component of island respectively, is entered through feeding system respective
It melted by heating and is squeezed out in screw extruder, forms spinning melt using respective fondant filter, finally enter manifold
Carry out spinning；
Spinning melt into manifold initially enters respective metering pump and is measured according to the ratio of island component,
The mass ratio control in middle sea, island component is 30%:37 island 70%, island Shuo Wei, subsequently into composite spining module, finally by spinneret
Plate sprays, and forms island structure composite filament；
(3) cooling falls bucket：
The silk sprayed from spinneret is cooled and shaped by cross air blasting, after oiling and silk, by winding device formation fiber barrel；
(4) drawing-off crimps：
The tow of certain amount fiber barrel is passed through into creel boundling, then carries out drawing-off, drawing temperature is controlled at 150 DEG C,
Again into 120 DEG C of hot steam sizings are crossed, finally enters crimper and be crimped；
(5) dry cutting：
Tow after curling carries out the dryness finalization that relaxes, and finally determines the short fibre in island for what dried tow cut into 38mm.
Superfiber leather preparation example
A kind of preparation method of superfiber leather, includes the following steps：
(1) woven fabric：
The island ultrafine fiber that application examples is obtained carries out shredding, combing, lapping, forms composite layer fibre web, and fibre web passes through
Subsequent several needing machines carry out needle thorn, form needle punched non-woven fabrics；
(2) it impregnates：
Obtained non-woven cloth is impregnated by polyurethane solutions；
(3) it solidifies：
By the non-woven cloth after dipping concentration is 20%~50%, temperature is 20~50 DEG C of dimethylformamides (DMF)
It is sufficiently solidified in aqueous solution, setting time 30min-60min；
(4) it washes：
Synthetic leather immersed substrate is sufficiently washed in 40~70 DEG C of water；
(5) Alkali reduction：
The substrate of dipping is immersed in the NaOH solution that concentration is 15~30g/L, temperature is 80~100 DEG C, handles base
30~60min of material is removed and is determined sea component in the fiber of island, is allowed to realize the fine of fiber, then adequately washed, in
With；
(6) dry：Substrate after neutralization is dried in air oven, obtains the synthesis of graphene superfine fibre
Leather.
Performance test
The superfiber leather being prepared is performed the following performance tests：
(1) bacteria resistance：Test method is GB/T20944.3-2008《The evaluation third portion of antibacterial textile performance
Point：Succusion》, biomass graphene modified polyamine fibre and Fypro are determined respectively, and Escherichia coli, white are read
The bacteriostasis rate of pearl bacterium and staphylococcus aureus.
(2) temperature rise is tested, referring in particular to GB/T 30127-2013《The detection and evaluation of textile far infrared performance》.
(3) it is cracked：Test method is QB/T 3812.7《The measurement of grain side of leather intensity and stretching, extension height is burst apart test》
Test result is shown in Table 1.
Table 1 prepares the performance test of superfiber leather using the graphene composite master batch of embodiment and comparative example
As it can be seen from table 1 when mixing substrate by several times with grapheme material, and rear primary combined amount≤back base
When within the 10 of material combined amount, excellent antibacterial (staphylococcus aureus, Escherichia coli, Candida albicans) property can be obtained
Can, staphylococcus aureus biocidal property is 88% or more, and 86% or more, Candida albicans bacteriostasis rate exists Escherichia coli bacteriostasis rate
85% or more, cracking value is in 5mm or more, and heating rate is at 2 DEG C or more.
The Applicant declares that the present invention illustrates the process method of the present invention through the above embodiments, but the present invention not office
It is limited to above-mentioned processing step, that is, does not mean that the present invention must rely on the above process steps to be carried out.Technical field
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., all of which fall within the scope of protection and disclosure of the present invention.
Claims (10)
1. a kind of preparation method of graphene composite master batch, which is characterized in that the preparation method includes the following steps：
(1) substrate is divided into n parts, and the quality of (n+1)th part of substrate is less than 10 times of n-th part of substrate mass；
(2) the 1st part of substrate is mixed with grapheme material, obtains the 1st mixture；
(3) (n+1)th part of substrate is mixed with n-th mixture, obtains (n+1)th mixture, being granulated after melting is graphene
Composite master batch；
Wherein n takes positive integer.
2. preparation method as described in claim 1, which is characterized in that the preparation method includes the following steps：
(1) substrate is divided into 2 parts, and the quality of the 2nd part of substrate is less than 10 times of the 1st part of substrate mass；
(2) the 1st part of substrate is mixed with grapheme material, obtains the 1st mixture；
(3) the 2nd part of substrate is mixed with the 1st mixture, obtains the 2nd mixture, being granulated after melting is that graphene is compound
Master batch.
3. preparation method as claimed in claim 2, which is characterized in that step (2) grapheme material and the 1st part of substrate
Mass ratio is 1:10~100；
Preferably, step (2) mode for mixing the 1st part of substrate with grapheme material includes the following steps：
(2a) mixes the 1st part of substrate with the grapheme material of partial size D90≤1 μm；
(2b) mixes the mixed material of step (2a) with the grapheme material of 1 μm of D90≤8 μm < of partial size；
Preferably, the quality of the grapheme material of partial size D90≤1 μm and the grapheme material of 1 μm of D90≤8 μm < of partial size
Than being 1:1~5；
Preferably, in terms of by the gross mass of graphene composite master batch for 100 parts by weight, the quality of the grapheme material is 5~10
Parts by weight；
Preferably, the grapheme material includes graphene, any a kind or at least two kinds of of combination in Graphene derivative, excellent
Graphene, the gas for selecting redox graphene, graphene oxide, the graphene that biomass is raw material preparation, removing graphite to obtain
Mutually deposit any a kind or at least two kinds of of combination in obtained graphene；
Preferably, the substrate includes polypropylene fibre master batch, dacron master grain, chinlon master batch, spandex master batch, any 1 in acrylic fibers master batch
Kind or at least two kinds of combinations.
4. a kind of graphene composite master batch, which is characterized in that the graphene composite master batch passes through one of claims 1 to 3 institute
The preparation method stated is prepared.
5. a kind of preparation method of modified fibre, which is characterized in that the preparation method includes：
Graphene composite master batch as claimed in claim 4 and blank slice are mixed to get mixture, carry out spinning later；
Preferably, the component of the mixture includes following component in parts by weight：
5~15 parts of graphene composite master batch
Blank is sliced 85~95 parts
The sum of described mixture each component is 100 parts by weight；
Preferably, the partial size of the graphene composite master batch as claimed in claim 4 is less than or equal to the partial size of blank slice, preferably
The ratio between graphene composite master batch as claimed in claim 4 and the partial size of blank slice are 1:2~10.
6. a kind of preparation method for determining island sea-island composite fiber, which is characterized in that the preparation method includes the following steps：
Graphene composite master batch as claimed in claim 4 is added in the component of island, obtains being mixed with graphene composite master batch
Island component, then by sea component be mixed with the island component of graphene composite master batch melting mixing during melt spinning, it
After carry out spinning, obtain island fiber with figured sea-island；
Preferably, the island component for being mixed with graphene composite master batch includes following component in parts by weight：
5~15 parts of graphene composite master batch
85~95 parts of island component
The sum of described mixture each component is 100 parts by weight；
Preferably, the partial size of the graphene composite master batch as claimed in claim 4 is less than or equal to the partial size of island component, preference
Benefit require 4 described in the ratio between the partial size of graphene composite master batch and island component be 1:2~10；
Preferably, the mixed proportion of the sea component and the island component for being mixed with graphene composite master batch is 30%~40%:
70%~60%；
Preferably, 37 island island Shuo Wei for determining island sea-island composite fiber；
Optionally, it after " spinning " step, is oiled, drawing-off, drying steps.
7. a kind of determine island sea-island composite fiber, which is characterized in that described to determine island sea-island composite fiber by claim 6 institute
The preparation method stated is prepared.
8. a kind of preparation method of superfiber leather, which is characterized in that the preparation method includes the following steps：
(I) determined island sea-island composite fiber with as claimed in claim 7 and prepared non-woven fabrics；
(II) by the non-woven fabrics impregnating polyurethane solution of step (I)；
(III) non-woven fabrics after step (II) to be impregnated to polyamide solution solidifies in dimethylformamide in water, water
After washing, the sea component determined in the sea-island composite fiber of island is removed by Alkali reduction；
(IV) step (III) treated non-woven fabrics is dry, obtain superfiber leather；
Preferably, the concentration of step (III) described dimethylformamide in water is 20~50wt%；
Preferably, the temperature of the solidification is 20~50 DEG C, and the time is 30~60min；
Preferably, the temperature of the washing is 40~70 DEG C；
Preferably, the Alkali reduction, which removes, determines the mode of the sea component in the sea-island composite fiber of island and is：
Non-woven fabrics after washing is immersed in the NaOH solution that concentration is 15~30g/L, temperature is 80~100 DEG C, handles base
30~60min of material.
9. a kind of superfiber leather, which is characterized in that the superfiber leather is prepared by preparation method according to any one of claims 8
It obtains.
10. a kind of purposes of superfiber leather, which is characterized in that the superfiber leather is used to prepare shoes, luggage, furniture or vapour
In-car decorations.
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| CN109762305A (en) * | 2019-01-22 | 2019-05-17 | 宁波石墨烯创新中心有限公司 | A kind of graphene master batch and preparation method thereof |
| CN110886030A (en) * | 2019-12-20 | 2020-03-17 | 湖州拉杜拉塔服饰有限公司 | Preparation method of nylon yarn with good antibacterial and dyeing properties |
| CN114892413A (en) * | 2022-06-09 | 2022-08-12 | 吉安市三菱超细纤维有限公司 | Deodorizing and antibacterial functional synthetic leather and preparation method and application thereof |
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| CN105463598A (en) * | 2015-11-16 | 2016-04-06 | 四川大学 | Graphite-enhanced ultrafine synthetic leather fiber |
| CN105586658A (en) * | 2016-03-04 | 2016-05-18 | 济南圣泉集团股份有限公司 | Modified chinlon fiber, preparation method and application |
| KR20160138776A (en) * | 2015-05-26 | 2016-12-06 | 한국과학기술연구원 | Ultrafine carbon fibers and their preparation method |
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| KR20160138776A (en) * | 2015-05-26 | 2016-12-06 | 한국과학기술연구원 | Ultrafine carbon fibers and their preparation method |
| CN105463598A (en) * | 2015-11-16 | 2016-04-06 | 四川大学 | Graphite-enhanced ultrafine synthetic leather fiber |
| CN105586658A (en) * | 2016-03-04 | 2016-05-18 | 济南圣泉集团股份有限公司 | Modified chinlon fiber, preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109762305A (en) * | 2019-01-22 | 2019-05-17 | 宁波石墨烯创新中心有限公司 | A kind of graphene master batch and preparation method thereof |
| CN109762305B (en) * | 2019-01-22 | 2021-09-10 | 宁波石墨烯创新中心有限公司 | Graphene master batch and preparation method thereof |
| CN110886030A (en) * | 2019-12-20 | 2020-03-17 | 湖州拉杜拉塔服饰有限公司 | Preparation method of nylon yarn with good antibacterial and dyeing properties |
| CN114892413A (en) * | 2022-06-09 | 2022-08-12 | 吉安市三菱超细纤维有限公司 | Deodorizing and antibacterial functional synthetic leather and preparation method and application thereof |
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| CN108929446B (en) | 2021-07-06 |
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