CN107237120A - A kind of fibre maceration extract, modified fibre product and preparation method - Google Patents
A kind of fibre maceration extract, modified fibre product and preparation method Download PDFInfo
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- CN107237120A CN107237120A CN201710555625.8A CN201710555625A CN107237120A CN 107237120 A CN107237120 A CN 107237120A CN 201710555625 A CN201710555625 A CN 201710555625A CN 107237120 A CN107237120 A CN 107237120A
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- 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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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/144—Alcohols; Metal alcoholates
- D06M13/148—Polyalcohols, e.g. glycerol or glucose
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/35—Heterocyclic compounds
- D06M13/355—Heterocyclic compounds having six-membered heterocyclic rings
- D06M13/358—Triazines
- D06M13/364—Cyanuric acid; Isocyanuric acid; Derivatives thereof
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- 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
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
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- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
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- D06M2101/16—Synthetic fibres, other than mineral fibres
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- D06M2101/16—Synthetic fibres, other than mineral fibres
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Abstract
The present invention relates to a kind of fibre maceration extract, functional components are dispersed with the fibre maceration extract, the functional components are the composition of grapheme material and bamboo charcoal.The present invention disperses the functional components that are made up of grapheme material and bamboo charcoal in maceration extract, and it can mutually be adsorbed, and reduces the reunion of graphene, add the specific surface area of bamboo charcoal, Synergistic antibiotic property and deodorization；In optimal technical scheme, at least part grapheme material is crosslinked with least part bamboo charcoal by chemical bond, realizes the purpose being firmly bonded to grapheme material on bamboo charcoal, plays enhancing specific surface area, strengthens the effect of the adsorption capacity of bamboo charcoal.
Description
Technical field
The invention belongs to fibre technology field, more particularly to a kind of fibre maceration extract, modified fibre product and preparation
Method.
Background technology
In order to assign fibre (such as fabric, fiber) some different additional functions, such as conduction, antistatic, anti-spoke
Penetrate, soft, deodorization etc., impregnation process can be carried out to fibre from maceration extract.For different additional functions, maceration extract
In can add corresponding functional components.
Bamboo charcoal is mainly made up of elements such as charcoal, hydrogen, oxygen, and quality is hard, fine and closely woven porous, high adsorption capacity, its adsorption capacity
It is more than 10 times of same volume charcoal, contained mineral matter is more than 5 times of same volume charcoal, therefore there is good deodorization, prevent
Rotten, absorption peculiar smell function.Nano bamboo micro mist also has effects that good antibacterial, sterilization, can adsorb and neutralize sweat
Acidic materials contained by liquid, reach effect of skin whitening.Moreover, bamboo charcoal or well far infrared and anion
Emissive material.
But need to add many other auxiliary elements (for example in the prior art, in the maceration extract containing bamboo charcoal outward
The simple substance of the elements such as titanium, germanium, cerium, silicon, zinc, iron, zirconium, nickel or the nano particle of oxide), assign the maceration extract conductive, anti-
The effects such as electrostatic, radiation-proof antibacterial deodorizing, but these auxiliary element particle diameters and performance are complicated, it is difficult to it is uniformly dispersed.
This area needs to develop a kind of fibre maceration extract, and it can have the effects such as antistatic, antibacterial, deodorization,
It is uniformly dispersed simultaneously, and storage stability is good.
The content of the invention
In view of the shortcomings of the prior art, an object of the present invention is to provide a kind of fibre maceration extract, the fibre
Functional components are dispersed with fiber products maceration extract, the functional components are the composition of grapheme material and bamboo charcoal.
In the maceration extract, its functional components contained is grapheme material and bamboo charcoal grapheme material and bamboo charcoal energy
Enough mutually absorption, the particle diameter of grapheme material is much smaller compared with bamboo charcoal particle diameter, and it can be adsorbed on the surface of the bamboo charcoal, reduced certainly
Body is reunited, while bamboo charcoal is in itself due to having adsorbed grapheme material, add specific surface area, Synergistic antibiotic property and deodorization
Property.
Preferably, in the functional components, at least part grapheme material is handed over at least part bamboo charcoal by chemical bond
Connection.
Grapheme material and bamboo charcoal are by chemical bond cross-linked phase compared with Van der Waals force, and chemical bond crosslinking is more firm, with bamboo
The grapheme material of Carbon Materials strong bonded imparts the higher specific surface area of bamboo charcoal material.The graphite of chemical bonds will be passed through
Alkene material and bamboo charcoal are dispersed in maceration extract, and grapheme material is firmly adsorbed around bamboo charcoal particle by chemical bond, and many
Individual (more than 2) bamboo charcoal particle may also mutually be adsorbed by grapheme material each other, so that the chemical bonded refractory
The grapheme material and bamboo charcoal of conjunction have the big grain diameter of particle diameter, and this change reduces graphene, bamboo charcoal particle in dipping
Reunion in liquid, adds its dispersing uniformity, and it is the next ratio of substrate tape preferably to improve grapheme material and bamboo charcoal particle
The increase of surface area, and far-infrared anti-biotic performance raising.
Preferably, the particle diameter of the functional components is below 3 μm, such as 2.8 μm, 2.5 μm, 2.2 μm, 1.8 μm, 1.5 μ
M, 1.2 μm, 0.8 μm, preferably 0.5 μm, 0.2 μm etc., less than 1 μm.
Preferably, in the fibre maceration extract, the concentration of functional components is 0.05~2wt%, for example
0.08wt%, 0.10wt%, 0.12wt%, 0.25wt%, 0.36wt%, 0.45wt%, 0.60wt%, 0.85wt%,
0.93wt%, 1.10wt%, 1.12wt%, 1.25wt%, 1.36wt%, 1.45wt%, 1.60wt%, 1.85wt%,
1.93wt% etc..
Preferably, in the functional components, the mass ratio of grapheme material and bamboo charcoal is 1~99:99~1, such as 2:
98、5:95、10:90、15:85、20:80、25:75、30:70、35:65、40:60、45:55、50:50、55:45、60:40、65:
35、70:30、75:25、80:20、85:15、90:10、95:5 etc., preferably 100:1~20；
Preferably, the pH value of the fibre maceration extract is 7~11, such as 8,9,10.
The two of the object of the invention are to provide a kind of preparation method of the fibre maceration extract as described in the first purpose, described
Method comprises the following steps：
(A1) grapheme material is scattered in the alkaline aqueous solution that pH is 7~11；
(A2) bamboo charcoal is added in the solution that step (1) is obtained, ultrasonic disperse.
Preferably, the mass ratio of the grapheme material and bamboo charcoal is 1~99:99~1, such as 2:98、5:95、10:90、
15:85、20:80、25:75、30:70、35:65、40:60、45:55、50:50、55:45、60:40、65:35、70:30、75:
25、80:20、85:15、90:10、95:5 etc., preferably 100:1~20.
The three of the object of the invention are to provide the preparation method of another fibre maceration extract as described in the first purpose, institute
The method of stating comprises the following steps：
(B1) bamboo charcoal is activated, obtains the bamboo charcoal for being modified with oxygen-containing functional group；Then oxygen-containing functional group will be modified with
Bamboo charcoal mixed with grapheme material, add crosslinking agent, cross-linked polymeric；
(B2) product for obtaining step (B1) is scattered in the alkaline aqueous solution that pH is 7~11, ultrasonic disperse.
In the preparation method of fibre maceration extract of the present invention, " the production that step (B1) is obtained described in step (B2)
Thing " is the product of cross-linked polymeric, can will crosslink the liquid after polymerization and dry acquisition, drying means is not specifically limited,
Can by after spray drying, filtering by methods such as filtration cakes torrefactions.The drying steps preferably wash to neutral in reaction solution or
Carried out after alkalescence.
Preferably, the mass ratio of step (B1) bamboo charcoal and grapheme material is 100:1~20, such as 100:3、100:
4、100:6、100:8、100:10、100:12、100:15、100:16、100:18、100:19 etc., such as 100:2、100:3、
100:4、100:5、100:6、100:7、100:8、100:9、100:10、100:11、100:12、100:13、100:14、100:
15、100:16、100:17、100:18、100:19 etc., preferably 100:1~10, more preferably 100:1~5.
Preferably, restoring operation is carried out after step (1) described cross-linked polymeric.
Preferably, the reduction includes chemical reduction method, charing reducing process or Microwave reduction method.
Preferably, the chemical reduction method is is reduced using chemical reducing agent, and the chemical reducing agent includes hydration
Any a kind or at least two kinds of of combination in hydrazine, L-AA, sodium borohydride, sodium citrate, sodium hydroxide.
Preferably, the charing reducing process is carbonized under non-oxidizing atmosphere, the carbonization temperature for 500~
1000 DEG C, carbonization time is 0.5~6h.
Preferably, the Microwave reduction method is carries out microwave reduction under non-oxidizing atmosphere, and microwave power is 5.1~
0.7kW, such as 5.2kW, 4.8kW, 4.5kW, 4.2kW, 3.8kW, 3.5kW, 3.2kW, 4.8kW, 4.5kW, 4.2kW, 0.8kW
It is 1~15min Deng, microwave time, such as 2min, 5min, 7min, 8min, 9min, 10min, 11min, 14min, microwave is also
Former temperature is 800~1200 DEG C, such as 850 DEG C, 900 DEG C, 950 DEG C, 1000 DEG C, 1050 DEG C, 1150 DEG C.
The present invention is not specifically limited to the source of bamboo charcoal, and the bamboo charcoal that any those skilled in the art result in can use
In the present invention, it can also can be prepared by commercially available by any method that can be known.
Preferably, the carbon source of the bamboo charcoal includes bamboo material, preferably includes mao bamboon and/or bamboo.
Grapheme material of the present invention is any material with graphene sheet layer that those skilled in the art can be known
Material, including graphene, graphene oxide, functional group's graphite alkene etc..For the preparation method of the grapheme material, the present invention
It is not specifically limited, the method that can be peeled off by graphite, the method reduced after graphite oxide, method of chemical vapor deposition etc.
Deng.
Preferably, the grapheme material is the material with graphene film Rotating fields, preferably includes graphene, oxidation stone
Any a kind or at least two kinds of of combination in black alkene, Graphene derivative.
Preferably, the graphene includes peeling off graphene that graphite prepares, prepared by redox graphene
Obtained graphene, by reducing the graphene prepared after graphite oxide, being obtained by chemical vapor deposition carbonaceous gas
Graphene, any a kind or at least two kinds of of combination in the graphene that is obtained by Pintsch process biomass material.
Preferably, the step of " being activated bamboo charcoal " described in step (B1) includes：Bamboo charcoal is mixed with activator.
Preferably, the activator includes oxidant, appointing preferably in nitric acid, sulfuric acid, phosphoric acid, sodium hypochlorite, hydrogen peroxide
The combination of a kind or at least two kinds of of meaning.
Preferably, the addition of the activator is 0.1~10 times of bamboo charcoal weight, such as 0.5 times, 0.7 times, 1.3 times,
1.8 times, 2.3 times, 2.8 times, 3.3 times, 3.8 times, 4.3 times, 4.8 times, 5.3 times, 5.8 times, 6.3 times, 6.8 times, 7.3 times, 7.8
Again, 8.3 times, 8.8 times, 9.3 times, 9.8 times etc..
Preferably, the temperature of the activation be 35~85 DEG C, such as 35 DEG C, 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C, 65
DEG C, 70 DEG C, 75 DEG C, 80 DEG C, 85 DEG C etc., the soak time be 0.5~10h, such as 0.6h, 1.2h, 1.7h, 2.2h, 2.7h,
3.2h, 3.7h, 4.2h, 4.7h, 5.2h, 5.7h, 6.2h, 6.7h, 7.2h, 7.7h, 8.2h, 8.7h, 9.2h, 9.7h etc..
Preferably, step (B1) described crosslinking agent includes ethylene glycol, polyethylene glycol, propane diols, polypropylene glycol, fourth two
Any 1 in alcohol, ring pentanediol, cyclohexanediol, monoethanolamine, ethylenediamine, aliphatic diamine, melamine, two mercaptan, mercaptoethanol
Plant or at least two kinds of combinations；
Preferably, the addition of the crosslinking agent is 0.1~10 times of grapheme material weight, such as 0.5 times, 0.7 times,
1.3 times, 1.8 times, 2.3 times, 2.8 times, 3.3 times, 3.8 times, 4.3 times, 4.8 times, 5.3 times, 5.8 times, 6.3 times, 6.8 times, 7.3
Again, 7.8 times, 8.3 times, 8.8 times, 9.3 times, 9.8 times etc..
Preferably, the pH value of the cross-linked polymeric is 4~8, such as 5,6,7, and the temperature of cross-linked polymeric is 30~90 DEG C,
Such as 35 DEG C, 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C, 70 DEG C, 75 DEG C, 80 DEG C, 85 DEG C, the time is 0.5~12h,
Such as 0.6h, 1.2h, 1.7h, 2.2h, 2.7h, 3.2h, 3.7h, 4.2h, 4.7h, 5.2h, 5.7h, 6.2h, 6.7h, 7.2h,
7.7h, 8.2h, 8.7h, 9.2h, 9.7h, 10h, 11h etc..
The three of the object of the invention are to provide a kind of modified fibre product, and the modified fibre product is by impregnating described in purpose
Maceration extract be modified.
Preferably, the fibre includes any a kind or at least two kinds of of combination in fiber, yarn, fabric, fabric.
Preferably, the fiber include polyester fiber, nylon fibre, acrylic fiber and polypropylene fiber in any a kind or
At least two kinds of combinations.
Preferably, the yarn is single yarn and/or scribbled.
The four of the object of the invention are to provide a kind of preparation method of the modified fibre product as described in the third purpose, the side
Method includes：Unmodified fibre is impregnated in the maceration extract described in the first purpose, afterwards through supercooling, drying, obtained
Modified fibre product.
Preferably, the dipping temperature is 60~90 DEG C, such as 65 DEG C, 70 DEG C, 75 DEG C, 80 DEG C, 85 DEG C, dip time
For 15~100min, such as 20min, 25min, 30min, 35min, 40min, 45min, 50min, 55min, 60min, 65min,
70min, 75min, 80min, 85min, 90min, 95min etc..
Preferably, when the maceration extract 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 into maceration extract.
Preferably, the addition of the reducing agent be graphene oxide 10~200wt%, such as 15wt%, 22wt%,
27wt%, 33wt%, 38wt%, 44wt%, 58wt%, 65wt%, 80wt%, 98wt%, 103wt%, 120wt%,
135wt%, 155wt%, 165wt%, 187wt%, 195wt% etc., preferably 50~100wt%.
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；It is described heating reduction temperature≤200 DEG C, such as 180 DEG C, 150 DEG C, 130 DEG C, 100 DEG C, 80 DEG C, 50
DEG C etc., pressure≤1.6MPa, such as 1.5MPa, 1.4MPa, 1.3MPa, 1.2MPa, 1.1MPa, 1.0MPa, 0.9MPa,
0.8MPa, 0.7MPa, 0.6MPa, 0.5MPa etc..
The five of the object of the invention are to provide a kind of purposes of the modified fibre product as described in the third purpose, described modified fine
Fiber products are used as preparing any a kind or at least two kinds of of combination in clothes, exposure suit.
Compared with prior art, the present invention has the advantages that：
(1) present invention disperses the functional components being made up of grapheme material and bamboo charcoal in maceration extract, and it can be mutual
Absorption, reduce the reunion of graphene, add the specific surface area of bamboo charcoal, Synergistic antibiotic property and deodorization；
(2) in optimal technical scheme, at least part grapheme material is crosslinked with least part bamboo charcoal by chemical bond, real
Show the purpose being firmly bonded to grapheme material on bamboo charcoal, played enhancing specific surface area, strengthen the adsorption capacity of bamboo charcoal
Effect.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is only to aid in understanding the present invention, is not construed as the concrete restriction to the present invention.
Embodiment 1
A kind of maceration extract, preparation method comprises the following steps：
(1) 10g bamboo charcoals (D90=3 μm) are dispersed in 500mL 0.1M sulfuric acid solutions, 1h are stirred at 80 DEG C, so
Precipitation cleaning is activated to pH close to 7 afterwards, Activated Bamboo is obtained；Then Activated Bamboo is dispersed in 100mL 1wt%
In glycol water, then in instillation 0.5wt% graphene oxide water solutions under 80 DEG C of counterflow conditions, and continue to stir 12h,
Cross-linked polymeric is carried out, dries, obtains functional components；In the functional components, the mass ratio of bamboo charcoal and graphene oxide is
100:10；
(2) functional components are scattered in the alkaline aqueous solution that pH is 7~11, ultrasonic disperse obtains maceration extract.
Embodiment 2
Difference with embodiment 1 is that step (1) is：
10g bamboo charcoals (D90=3 μm) are dispersed in 500mL 0.1M sulfuric acid solutions, 1h is stirred at 80 DEG C, then will
Precipitation cleaning is activated to pH close to 7, obtains Activated Bamboo；Then Activated Bamboo is dispersed in 100mL 1wt% second two
In alcohol solution, then in instillation 0.5wt% graphene oxide water solutions under 80 DEG C of counterflow conditions, and continue to stir 12h, carry out
Cross-linked polymeric；5mL 20wt% hydrazine hydrates are added afterwards, then will be precipitated with deionized water and be cleaned constant to washing lotion electrical conductivity,
It will finally be ground after 80 DEG C of dryings of filter cake, obtain functional components；In the functional components, the mass ratio of bamboo charcoal and graphene
For 100:10.
Embodiment 3
A kind of maceration extract, preparation method comprises the following steps：
(1) 5g bamboo charcoals (D90=2 μm) are dispersed in 500mL 0.1M sulfuric acid solutions, 5h are stirred at 80 DEG C, then
By precipitation cleaning to pH close to 7, activated, obtain Activated Bamboo；Then Activated Bamboo is dispersed in 100mL 10wt% second
In two alcohol solutions, then in instillation 0.5wt% graphene oxide water solutions under 80 DEG C of counterflow conditions, and continue to stir 12h, enter
Row cross-linked polymeric, dries, obtains functional components；In the functional components, the mass ratio of bamboo charcoal and graphene oxide is
100:1；
(2) functional components are scattered in the alkaline aqueous solution that pH is 7~11, ultrasonic disperse obtains maceration extract.
Embodiment 4
Difference with embodiment 3 is that step (1) is：
5g bamboo charcoals (D90=2 μm) are dispersed in 500mL 0.1M sulfuric acid solutions, 5h is stirred at 80 DEG C, then will
Precipitation cleaning is activated to pH close to 7, obtains Activated Bamboo；Then Activated Bamboo is dispersed in 100mL 10wt% second two
In alcohol solution, then in instillation 0.5wt% graphene oxide water solutions under 80 DEG C of counterflow conditions, and continue to stir 12h, carry out
Cross-linked polymeric；Afterwards by the product of cross-linked polymeric in 60 DEG C of constant temperature dryings, then it is placed in the lower 1000 DEG C of microwave treatments of nitrogen protection
60min is reduced, then with deionization by microwave reduction product cleaning to filtrate stable conductivity, finally by filter cake 80 DEG C do
Ground after dry, obtain functional components；In the functional components, the mass ratio of bamboo charcoal and graphene oxide is 100:1.
Embodiment 5
A kind of maceration extract, preparation method comprises the following steps：
(1) 5g bamboo charcoals (less than 1 μm) are dispersed in 500mL 0.1M phosphoric acid solutions, 5h are stirred at 40 DEG C, then
By precipitation cleaning to pH close to 7, activated, obtain Activated Bamboo；Then Activated Bamboo is dispersed in 100mL 10wt% tri-
In paracyanogen amine aqueous solution, then in instillation 0.5wt% graphene oxide water solutions under 80 DEG C of counterflow conditions, and continue to stir 12h,
Cross-linked polymeric is carried out, dries, obtains functional components；In the functional components, the mass ratio of bamboo charcoal and graphene oxide is
100:20；
(2) functional components are scattered in the alkaline aqueous solution that pH is 7~11, ultrasonic disperse obtains maceration extract.
Embodiment 6
Difference with embodiment 1 is, during the activator of step (1) is liquor natrii hypochloritis, the liquor natrii hypochloritis
The quality of sodium hypochlorite is 10g, and activation temperature is 35 DEG C, and the time is 10h.
Embodiment 7
Difference with embodiment 1 is that the activator of step (1) is the matter of nitric acid in salpeter solution, the salpeter solution
Measure as 50g, activation temperature is 50 DEG C, and the time is 1h.
Embodiment 8
Difference with embodiment 1 is that the activator of step (1) is the matter of sulfuric acid in salpeter solution, the salpeter solution
Measure as 10g, activation temperature is 50 DEG C, and the time is 1h.
Embodiment 9
Difference with embodiment 1 is that the 100mL of step (1) 10wt% glycol waters replace with 100mL's
50wt% glycol waters, cross-linked polymeric temperature is 30 DEG C, and the time is 3h.
Embodiment 10
Difference with embodiment 1 is that the difference of step (1) is, the particle diameter of bamboo charcoal is 1~10 μm.
Embodiment 11
A kind of maceration extract, preparation method comprises the following steps：
(1) by 1g by reducing the graphene dispersion prepared after graphite oxide in the sodium hydroxide water that pH is 7~11
In solution；
(2) in the solution for obtaining (D90=3 μm) addition step (1) of 10g bamboo charcoals, ultrasonic disperse.
Comparative example 1
A kind of maceration extract, preparation method comprises the following steps：
(1) 10g bamboo charcoals (D90=3 μm) are dispersed in 500mL 0.1M sulfuric acid solutions, 1h are stirred at 80 DEG C, so
Precipitation cleaning is activated to pH close to 7 afterwards, Activated Bamboo is obtained；
(2) Activated Bamboo is scattered in the alkaline aqueous solution that pH is 7~11, ultrasonic disperse obtains maceration extract.
Comparative example 2
A kind of maceration extract, preparation method comprises the following steps：
(1) 10g bamboo charcoals (D90=3 μm) are scattered in the alkaline aqueous solution that pH is 7~11, ultrasonic disperse is impregnated
Liquid.
Comparative example 3
A kind of maceration extract, preparation method comprises the following steps：
(1) 1g graphene oxides are scattered in the alkaline aqueous solution that pH is 7~11, ultrasonic disperse obtains maceration extract.
Application examples 1~14
By unmodified fibre at 60~90 DEG C, be immersed in embodiment 1~14 offer maceration extract in 15~
100min, afterwards through supercooling, drying, obtains modified fibre product.
Application examples 15
By unmodified fibre at 60~90 DEG C, 15~100min in the maceration extract of the offer of embodiment 1 is immersed in,
Afterwards through supercooling, drying, it is placed in nitrogen and protects lower 1000 DEG C of microwave treatment 60min to be reduced, dry, be modified afterwards
Fibre.
Blank example
By unmodified fibre at 60~90 DEG C, be immersed in pH be 7~11 alkaline aqueous solution in 15~
100min, afterwards through supercooling, drying, obtains blank sample.
Performance test
Far infrared heating test and antibacterial bacteriostatic test are carried out to the gained fiber of application examples 1~15, method of testing is as follows：
Far-infrared temperature rise detection method：GB/T 30127-2013《The detection and evaluation of textile far infrared performance》；
Antibacterial bacteriostatic detection method：GB/T 20944.3-2008《The evaluation of antibacterial textile performance》.
Test result is as shown in table 1：
The performance test results of the application examples 1~15 of table 1
From the performance test results as can be seen that respectively with Activated Bamboo (application examples 12), bamboo charcoal (application examples 13) and oxidation
Graphene (application examples 14) is scattered to be obtained maceration extract fibre is impregnated, its wash 20 times after substantially no longer with antibacterial
Performance, it can be seen that its adhesive force on fibre is excessively poor, and by grapheme material and bamboo charcoal collectively as function material
Material, both mutually cooperate with, and improve absorption affinity of the functional components on fibre in maceration extract, when washing 50 times still
Good far infrared performance and anti-microbial property (more than 85%) can be kept；Especially when bamboo charcoal is crosslinked with grapheme material
Functional components afterwards ensure that bamboo charcoal and graphene Synergistic far infrared performance and anti-microbial property, additionally it is possible to improve washable
The ability washed, after 50 times are washed, anti-microbial property is not decreased obviously.
Applicant states that the present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological process, that is, do not mean that the present invention has to rely on above-mentioned detailed
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
Addition, selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., all fall within the present invention's
Within the scope of protection domain and disclosure.
Claims (10)
1. a kind of fibre maceration extract, it is characterised in that be dispersed with functional components in the fibre maceration extract, described
Functional components are the composition of grapheme material and bamboo charcoal.
2. fibre maceration extract as claimed in claim 1, it is characterised in that in the functional components, at least part stone
Black alkene material is crosslinked with least part bamboo charcoal by chemical bond；
Preferably, the particle diameter of the functional components is below 3 μm, preferably less than 1 μm；
Preferably, in the fibre maceration extract, the concentration of functional components is 0.05~2wt%；
Preferably, in the functional components, the mass ratio of grapheme material and bamboo charcoal is 1~99:99~1, preferably 100:1~
20；
Preferably, the pH value of the fibre maceration extract is 7~11.
3. a kind of preparation method of fibre maceration extract as claimed in claim 1 or 2, it is characterised in that methods described bag
Include following steps：
(A1) grapheme material is scattered in the alkaline aqueous solution that pH is 7~11；
(A2) bamboo charcoal is added in the solution that step (1) is obtained, ultrasonic disperse；
Preferably, the mass ratio of the grapheme material and bamboo charcoal is 1~99:99~1, preferably 100:1~20.
4. a kind of preparation method of fibre maceration extract as claimed in claim 1 or 2, it is characterised in that methods described bag
Include following steps：
(B1) bamboo charcoal is activated, obtains the bamboo charcoal for being modified with oxygen-containing functional group；Then the bamboo of oxygen-containing functional group will be modified with
Charcoal is mixed with grapheme material, adds crosslinking agent, cross-linked polymeric；
(B2) product for obtaining step (B1) is scattered in the alkaline aqueous solution that pH is 7~11, ultrasonic disperse；
Preferably, the mass ratio of step (B1) bamboo charcoal and grapheme material is 100:1~20, preferably 100:1~10, it is more excellent
Select 100:1~5；
Preferably, restoring operation is carried out after step (1) described cross-linked polymeric；
Preferably, the reduction includes chemical reduction method, charing reducing process or Microwave reduction method；
Preferably, the chemical reduction method is is reduced using chemical reducing agent, and the chemical reducing agent includes hydrazine hydrate, L-
Any a kind or at least two kinds of of combination in ascorbic acid, sodium borohydride, sodium citrate, sodium hydroxide；
Preferably, the charing reducing process is is carbonized under non-oxidizing atmosphere, and the carbonization temperature is 500~1000
DEG C, carbonization time is 0.5~6h；
Preferably, the Microwave reduction method is carries out microwave reduction under non-oxidizing atmosphere, and microwave power is 5.1~0.7kW,
The microwave time is 1~15min, and microwave reduction temperature is 800~1200 DEG C.
5. the preparation method of the fibre maceration extract as described in claim 3 or 4, it is characterised in that the carbon source of the bamboo charcoal
Including bamboo material, mao bamboon and/or bamboo are preferably included；
Preferably, the grapheme material is the material with graphene film Rotating fields, preferably includes graphene, graphite oxide
Any a kind or at least two kinds of of combination in alkene, Graphene derivative；
Preferably, the graphene includes peeling off graphene that graphite prepares, prepared by redox graphene
Graphene, the stone by reducing the graphene prepared after graphite oxide, being obtained by chemical vapor deposition carbonaceous gas
Any a kind or at least two kinds of of combination in black alkene, the graphene obtained by Pintsch process biomass material.
6. the preparation method of fibre maceration extract as claimed in claim 4, it is characterised in that " will described in step (B1)
Bamboo charcoal is activated " the step of include：Bamboo charcoal is mixed with activator；
Preferably, the activator includes oxidant, any a kind preferably in nitric acid, sulfuric acid, phosphoric acid, sodium hypochlorite, hydrogen peroxide
Or at least two kinds of combinations；
Preferably, the addition of the activator is 0.1~10 times of bamboo charcoal weight；
Preferably, the temperature of the activation is 35~85 DEG C, and the soak time is 0.5~10h；
Preferably, step (B1) described crosslinking agent includes ethylene glycol, polyethylene glycol, propane diols, polypropylene glycol, butanediol, ring
Any a kind in pentanediol, cyclohexanediol, monoethanolamine, ethylenediamine, aliphatic diamine, melamine, two mercaptan, mercaptoethanol or
At least two kinds of combinations；
Preferably, the addition of the crosslinking agent is 0.1~10 times of grapheme material weight；
Preferably, the pH value of the cross-linked polymeric is 4~8, and the temperature of cross-linked polymeric is 30~90 DEG C, and the time is 0.5~12h.
7. a kind of modified fibre product, it is characterised in that the modified fibre product is by impregnating described in claim 1 or 2
Maceration extract is modified；
Preferably, the fibre includes any a kind or at least two kinds of of combination in fiber, yarn, fabric, fabric；
Preferably, the fiber includes any a kind or at least 2 in polyester fiber, nylon fibre, acrylic fiber and polypropylene fiber
The combination planted；
Preferably, the yarn is single yarn and/or scribbled.
8. a kind of preparation method of modified fibre product as claimed in claim 7, it is characterised in that methods described includes：Will
Unmodified fibre impregnates in the maceration extract described in claim 1 or 2, afterwards through supercooling, drying, obtains modified fibre
Fiber products；
Preferably, the dipping temperature is 60~90 DEG C, and dip time is 15~100min.
9. the preparation method of modified fibre product as claimed in claim 8, it is characterised in that when the maceration extract includes oxygen
During graphite alkene, 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 into maceration extract；
Preferably, the addition of the reducing agent is the 10~200wt%, preferably 50~100wt% of graphene oxide；
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.
10. a kind of purposes of modified fibre product as claimed in claim 7, it is characterised in that the modified fibre product is used
Prepare any a kind or at least two kinds of of combination in clothes, exposure suit.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108035165A (en) * | 2017-12-21 | 2018-05-15 | 芜湖品度电子科技有限公司 | Mould-proof antibacterial braid and preparation method thereof |
| CN108486863A (en) * | 2018-04-24 | 2018-09-04 | 济南圣泉集团股份有限公司 | A kind of grapheme material modified fabric of antistatic and preparation method thereof |
| CN108729211A (en) * | 2018-07-10 | 2018-11-02 | 江苏红东科技有限公司 | The graphene that graphene is modified the preparation method of anti-bacterial fibre and is prepared is modified anti-bacterial fibre and gauze |
| CN110466214A (en) * | 2019-08-16 | 2019-11-19 | 广州哥伦布科技发展有限公司 | A kind of graphene fabric and preparation method thereof |
| CN111021050A (en) * | 2020-01-03 | 2020-04-17 | 深圳市寒暑科技新能源有限公司 | Antibacterial cotton fiber and preparation method thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103048372A (en) * | 2012-12-17 | 2013-04-17 | 同济大学 | Preparation method for biosensor based on graphene/carbon nano-tube |
| CN104599861A (en) * | 2014-12-31 | 2015-05-06 | 江苏江大环保科技开发有限公司 | Preparation method of graphene/xylogen-based active carbon |
| CN104947411A (en) * | 2015-07-07 | 2015-09-30 | 安徽理工大学 | Multifunctional fabric slurry composite and preparation method thereof |
| CN105220461A (en) * | 2015-10-30 | 2016-01-06 | 无锡市长安曙光手套厂 | A kind of multifunctional fabric slip composition and method of making the same |
| CN105603718A (en) * | 2016-02-05 | 2016-05-25 | 济南圣泉集团股份有限公司 | Composite fiber as well as preparation method and application thereof |
| CN106381716A (en) * | 2016-08-29 | 2017-02-08 | 徐杭婷 | Preparation method of fabric photochromic finishing liquid |
| CN106930098A (en) * | 2017-03-15 | 2017-07-07 | 山东圣泉新材料股份有限公司 | A kind of composite fibre, preparation method and its usage |
| CN106930099A (en) * | 2017-03-15 | 2017-07-07 | 山东圣泉新材料股份有限公司 | A kind of composite fibre, preparation method and its usage |
-
2017
- 2017-07-10 CN CN201710555625.8A patent/CN107237120A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103048372A (en) * | 2012-12-17 | 2013-04-17 | 同济大学 | Preparation method for biosensor based on graphene/carbon nano-tube |
| CN104599861A (en) * | 2014-12-31 | 2015-05-06 | 江苏江大环保科技开发有限公司 | Preparation method of graphene/xylogen-based active carbon |
| CN104947411A (en) * | 2015-07-07 | 2015-09-30 | 安徽理工大学 | Multifunctional fabric slurry composite and preparation method thereof |
| CN105220461A (en) * | 2015-10-30 | 2016-01-06 | 无锡市长安曙光手套厂 | A kind of multifunctional fabric slip composition and method of making the same |
| CN105603718A (en) * | 2016-02-05 | 2016-05-25 | 济南圣泉集团股份有限公司 | Composite fiber as well as preparation method and application thereof |
| CN106381716A (en) * | 2016-08-29 | 2017-02-08 | 徐杭婷 | Preparation method of fabric photochromic finishing liquid |
| CN106930098A (en) * | 2017-03-15 | 2017-07-07 | 山东圣泉新材料股份有限公司 | A kind of composite fibre, preparation method and its usage |
| CN106930099A (en) * | 2017-03-15 | 2017-07-07 | 山东圣泉新材料股份有限公司 | A kind of composite fibre, preparation method and its usage |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108035165A (en) * | 2017-12-21 | 2018-05-15 | 芜湖品度电子科技有限公司 | Mould-proof antibacterial braid and preparation method thereof |
| CN108486863A (en) * | 2018-04-24 | 2018-09-04 | 济南圣泉集团股份有限公司 | A kind of grapheme material modified fabric of antistatic and preparation method thereof |
| CN108729211A (en) * | 2018-07-10 | 2018-11-02 | 江苏红东科技有限公司 | The graphene that graphene is modified the preparation method of anti-bacterial fibre and is prepared is modified anti-bacterial fibre and gauze |
| CN108729211B (en) * | 2018-07-10 | 2023-11-17 | 江苏红东科技有限公司 | Preparation method of graphene modified antibacterial fiber and prepared graphene modified antibacterial fiber and gauze |
| CN110466214A (en) * | 2019-08-16 | 2019-11-19 | 广州哥伦布科技发展有限公司 | A kind of graphene fabric and preparation method thereof |
| CN110466214B (en) * | 2019-08-16 | 2021-12-31 | 广州骆驼家居家纺科技有限公司 | Graphene fabric and preparation method thereof |
| CN111021050A (en) * | 2020-01-03 | 2020-04-17 | 深圳市寒暑科技新能源有限公司 | Antibacterial cotton fiber and preparation method thereof |
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Application publication date: 20171010 |