CN108285540A - A kind of preparation method of aramid nano-fiber water-dispersed and aramid fiber nanometer paper - Google Patents
A kind of preparation method of aramid nano-fiber water-dispersed and aramid fiber nanometer paper 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
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/05—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media from solid polymers
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21F—PAPER-MAKING MACHINES; METHODS OF PRODUCING PAPER THEREON
- D21F11/00—Processes for making continuous lengths of paper, or of cardboard, or of wet web for fibre board production, on paper-making machines
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
- D21H13/10—Organic non-cellulose fibres
- D21H13/20—Organic non-cellulose fibres from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D21H13/26—Polyamides; Polyimides
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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
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino carboxylic acids or of polyamines and polycarboxylic acids
Abstract
The invention discloses the preparation methods of a kind of aramid nano-fiber water-dispersed and aramid fiber nanometer paper, aramid nano-fiber prepared by the present invention, can uniformly and stably it disperse in aqueous phase system or hydrophilic solvent completely, the method of the present invention preparation process flow is simple, short route is realized to prepare, is easy to control, suitable for industrialization production, solves the problems such as current aramid nano-fiber can only be homogeneously dispersed in highly basic/DMSO system, can not uniformly and stably be scattered in aqueous phase system, cannot preserve for a long time；Aramid nano-fiber is greatly expanded to apply with enhancing with water-soluble polymer and being blended for hydrophilic material.Aramid nano-fiber water-dispersed prepared by method described above of the present invention is aramid fiber nanometer paper prepared by raw material, have many advantages, such as that forming evenness is good, paper structure is fine and close, mechanical strength and compressive resistance are had excellent performance, can be used as High Performance Insulation material and be widely used in high-end electric insulation field.
Description
Technical field
The invention belongs to polymer nano materials and field of papermaking, and in particular to a kind of aramid nano-fiber water-dispersed and virtue
The preparation method of synthetic fibre nanometer paper.
Background technology
Para-aramid fiber (PPTA) is a kind of high intensity, high-modulus, insulating properties and the excellent high-performance of high temperature resistance
Synthetic fibers are the desirable feedstocks of protection and reinforcing material, are widely used in aerospace, national defence, telecommunications, petrochemical industry
Equal fields.Rigid chain knot of the high-strength high-temperature stability of para-aramid fiber from the pi-conjugated formation of π-inside its strand
The two-dimensional network shape structure of the dense regular of the effects that structure, molecule interchain hydrogen bond and Van der Waals power formation.But this structure
Feature leads to the defects of aramid fiber surface is smooth, active group is few, chemical inertness is stronger, leads to the bases such as aramid fiber and resin
The interface binding power of body is poor, limits it in high-performance composite reinforcing material, nano material, filtering material, biological medicine etc.
Application in value segment.
Aramid nano-fiber (Aramid Nanofibers, ANFs) as it is a kind of it is emerging in recent years have excellent performance it is poly-
Object nanofiber is closed, (such as nano-particle, nanotube, is received nano wire using most inorganic nano reinforcing materials with Material Field
Rice piece) it is similar, there is unique nano-scale structures, big draw ratio and specific surface area while remaining aramid fiber macroscopic view fibre again
Excellent mechanical property and heat resistance are tieed up, mechanical performance, electrical property and the light that conventional chemical fiber cannot achieve are brought for it
Performance is learned, a kind of " construction unit " of novel structure macrocomposite is become, plays important interface humidification,
There is huge application prospect in fields such as composite material, biology, medicine, electronics, the energy.
The preparation of aramid nano-fiber is the chemical bases proposed by Nicholas A.Kotov seminars of U.S. professor earliest
Molten method (Yang M, Cao K, Sui L, et al.Dispersions of aramid nanofibers:anew nanoscale
building block[J].Acs Nano,2011,5(9):6945-54.).By by aramid fiber and highly basic (KOH) and two
It is continuously stirred at ambient temperature 7-10 days after methyl sulfoxide (Dimethyl sulphoxide, DMSO) mixing, obtains homogeneous point
Dissipate stable ANFs/DMSO dispersion liquids.KOH/DMSO alkali systems can orient effectively by destroying macroscopical aramid fiber point
Hydrogen bond crosslinks effect between subchain, while so that the N-H keys on amido bond is broken and deprotonation formation nitrogen anion occurs, band is negative
The π-πconjugation power and intermolecular van der Waals interaction that the strand of charge is generated in electrostatic repulsion, phenyl ring and amido bond
Lower dispersion is simultaneously stabilized.
But aramid nano-fiber prepared by this method can only exist under highly basic/DMSO system, when containing matter in dispersion liquid
Sub- donor (when such as dispersion liquid becomes neutral or alkalescent), nitrogen anion regain hydrogen atom, hydrogen bond between aramid nano-fiber
It re-forms, fiber agglomerates again.Especially, when dispersion liquid is water, protonation can occur for a large amount of aramid nano-fiber also
It is former, it is easy to generate aggregation and form membranaceous or reunion shape sediment；Moreover, because the DMSO in ANFs/DMSO systems is in humidity
Air in be easy to absorb water, and be easy to happen protonation reduction form membranaceous or reunion shape sediment, so prepare aramid fiber
Nano-solution cannot stored for a long time.Therefore, the aramid nano-fiber solution that prepared by this method is strong there is that can only be scattered in
Alkali/DMSO system, the problems such as can not being uniformly and stably scattered in aqueous phase system, cannot preserving for a long time, significantly limit it
With the application in water-soluble polymer and hydrophilic material so that the aramid nano-fiber haveing excellent performance, which cannot achieve, to be significantly increased
Effect limits its application field.
For this problem, current main resolving ideas is to utilize the active function that compatible reaction can be carried out with nitrogen anion
Group's organic molecule (such as chloro- 1- pentynes of bromo propine, chloro propine, 5-, the bromo- 2- butine of 1-) is anti-with aramid nano-fiber
Answer, obtain the aramid nano-fiber of active function base, then by it with active water soluble high-molecular compound [such as poly- second two
Alcohol monomethyl ether trinitride (m-PEG-N3), polyethylene glycol oxide trinitride (PEO-N3) and polyacrylic acid trinitride (PA-N3)] it carries out
Reaction obtains the aramid nano-fiber with water soluble functional group, is scattered in water after removing solvent using freeze-drying
Aramid nano-fiber water-dispersed (patent No. 201410833596.3) is obtained in solution.But the solution that the patent proposes is done
There is also problems with for method：First, so that it is carried soluble small molecular or function by reaction on aramid nano-fiber surface
Group will certainly cause its intensity, modulus and heat resistance to decline；The second, multistep reaction method needs catalyst and under anaerobic
Reaction, preparation process and complex process；Third needs to be freeze-dried in preparation process, and energy consumption is big, is unfavorable for industrialized production.
Invention content
The purpose of the present invention is to provide the preparation method of a kind of aramid nano-fiber water-dispersed and aramid fiber nanometer paper, with gram
Take the problems of the above-mentioned prior art, the present invention solve current aramid nano-fiber can only be homogeneously dispersed in highly basic/
In DMSO system, the problems such as can not being uniformly and stably scattered in aqueous phase system, cannot preserve for a long time.
In order to achieve the above objectives, the present invention adopts the following technical scheme that：
A kind of preparation method of aramid nano-fiber water-dispersed, includes the following steps：
(1) para-aramid fiber, potassium hydroxide, dimethyl sulfoxide (DMSO) are placed in container, are dispersed with stirring, is scattered in
Aramid nano-fiber dispersion liquid under KOH/DMSO systems；
(2) the aramid nano-fiber dispersion liquid being scattered under KOH/DMSO systems that will be obtained in step (1) is made in stirring
Under, to its high-pressure injection deionized water, obtain being scattered in KOH/DMSO/H2Aramid nano-fiber in O mixed systems；
(3) it is scattered in KOH/DMSO/H by what is obtained in step (2)2Aramid nano-fiber in O mixed systems passes through true
Sky filters, and obtains aramid nano-fiber；
(4) aramid nano-fiber obtained in step (3) is washed repeatedly by absolute ethyl alcohol and deionized water, obtains glue
Body shape aramid nano-fiber；
(5) the colloidal aramid nano-fiber obtained in step (4) is scattered in deionized water or parent under stirring
In aqueous solvent, aramid nano-fiber water-dispersed is obtained.
Further, para-aramid fiber, potassium hydroxide and dimethyl sulfoxide (DMSO) ratio are 1g in step (1)：1.5g：
500ml, the para-aramid fiber are p-aramid fiber yarn fibers, p-aramid fiber chopped strand, para-aramid pulp fiber
With one kind in p-aramid fiber fibrid.
Further, the high-pressure injection described in step (2) be utilize stainless steel high-pressure spray pump, jet pressure be 5~
15MPa, effluxvelocity are 0.2~2.0mL/s；The mass ratio of jet stream deionized water and para-aramid fiber is 1:1~5:1.
Further, the filter membrane that vacuum filtration uses in step (3) is 200~500 mesh nylon leaching film.
Further, the volume of washing absolute ethyl alcohol and the ratio of aramid fiber quality are 1mL in step (4):5mg~
1mL:2mg；The mass ratio of the washing deionized water and aramid fiber is 10:1~5:1.
Further, hydrophilic solvent is methanol, ethyl alcohol, propyl alcohol or isopropanol, and colloidal aramid fiber Nanowire in step (5)
It is 0.5~5mg/mL to tie up the dispersion concentration in deionized water or hydrophilic solvent.
Further, stirring refers to being stirred 5~8 days at a temperature of 30~50 DEG C under air-proof condition in step (1)；Step
Suddenly speed of agitator is 600~3000rpm in (2)；In step (5) agitation revolution be 500~2500rpm, mixing time 30~
180min。
A method of aramid fiber nanometer paper is prepared using aramid nano-fiber water-dispersed, is included the following steps：
(1) disperse：Aramid nano-fiber water-dispersed is scattered in deionized water and obtains aramid nano-fiber slurry, is disperseed
A concentration of 0.2~5mg/mL；
(2) Top wire former：The aramid nano-fiber slurry that step (1) obtains forming of manufacturing paper with pulp on oblique net paper machine is obtained into virtue
Synthetic fibre nanometer paper l Water Paper, forming quality a concentration of 0.02%~0.06%；
(3) drying is squeezed：The aramid fiber nanometer paper l Water Paper that step (2) obtains is placed in squeezer to squeeze and be dried to obtain aramid fiber
Nanometer paper body paper.
Further, condition is squeezed described in step (3) is：0.2~1.0MPa of squeeze pressure, the squeezing time 3~
20min；The drying condition is：Drying temperature：90~110 DEG C, 5~15min of drying time.
Compared with prior art, the present invention has technique effect beneficial below：
Aramid nano-fiber water-dispersed prepared by the present invention, solving current aramid nano-fiber can only be homogeneously dispersed in
In highly basic/DMSO system, the problems such as can not being uniformly and stably scattered in aqueous phase system, cannot preserve for a long time；It solves existing
There is technology so that it is declined with intensity, modulus and heat resistance caused by soluble small molecular or functional group by reaction, with
And the shortcomings of existing technology of preparing severe reaction conditions, preparation process and complex process.
Aramid nano-fiber water-dispersed prepared by the method for the present invention, can uniformly and stably be dispersed in aqueous phase system or parent
In aqueous solvent, and aramid nano-fiber good stability of the dimension, film strength are high, Good Heat-resistance, preparation process flow letter
It is single, it realizes short route and prepares, is easy to control, be suitable for industrialization production, be greatly expanded aramid nano-fiber and water-soluble poly
The blending for closing object and hydrophilic material is applied with enhancing.
The method of the present invention prepare aramid nano-fiber water-dispersed, due to its can be formed in aqueous phase system completely it is uniform
Steadily suspension, therefore, aramid nano-fiber water-dispersed prepared by method described above of the present invention are that aramid fiber prepared by raw material is received
Rice paper has many advantages, such as that forming evenness is good, paper structure is fine and close, mechanical strength and compressive resistance are had excellent performance, and without tradition
Hot-pressing processing technique needed for aramid paper production process, preparation flow is simple, low energy consumption, and it is extensive to can be used as High Performance Insulation material
Applied to electric insulation field, realizes that electric insulation equipment volume is small, capacity is big, promote the upgrading of electric insulation industry product and skill
Art progress.
The present invention adopts new technology, new method research and development have excellent performance aramid nano-fiber water-dispersed and utilize its preparation
Aramid fiber nanometer paper solves technical barrier of the existing technology and product disadvantage, strong innovation, excellent product performance, application
It has a extensive future, to pushing the Hi-tech Industry Developments such as composite material, promotes the upgrading of conventional industries, promote product shelves
It is secondary, promote the development of related industry, industry that there is certain realistic meaning.
Description of the drawings
Fig. 1 is PPTA molecular structural formulas and intermolecular hydrogen bonding combination schematic diagram；
Fig. 2 is the aramid fiber nanometer paper surface SEM image that the embodiment of the present invention 6 obtains.
Specific implementation mode
Embodiments of the present invention are described in further detail below：
A kind of preparation method of aramid nano-fiber water-dispersed, including following preparation process：
(1) para-aramid fiber, potassium hydroxide (KOH), dimethyl sulfoxide (DMSO) (DMSO) are placed in container, are dispersed with stirring,
Obtain the aramid nano-fiber dispersion liquid being scattered under KOH/DMSO systems；
Wherein, para-aramid fiber, KOH and DMSO ratios are 1g：1.5g：500mL；The stirring refers in sealing strip
Under part, stirred 5~8 days at a temperature of 30~50 DEG C；The para-aramid fiber is p-aramid fiber yarn fibers, p-aramid fiber
One kind in chopped strand, para-aramid pulp fiber and p-aramid fiber fibrid；
(2) the aramid nano-fiber dispersion liquid being scattered under KOH/DMSO systems that will be obtained in step (1) is made in stirring
Under, to its high-pressure injection deionized water, obtain being scattered in KOH/DMSO/H2Aramid nano-fiber in O mixed systems；
Wherein, stirring action stirs for high shear force, and speed of agitator is 600~3000rpm；The high-pressure injection is profit
With stainless steel high-pressure spray pump, jet pressure is 5~15MPa, and effluxvelocity is 0.2~2.0mL/s；The jet stream deionization
The mass ratio of water and aramid fiber is 1:1~5:1；
(3) it is scattered in KOH/DMSO/H by what is obtained in step (2)2Aramid nano-fiber in O mixed systems passes through true
Sky filters, and obtains aramid nano-fiber；
Wherein, the filter membrane used is filtered by vacuum as 200~500 mesh nylon leaching films；
(4) aramid nano-fiber obtained in step (3) is washed repeatedly by absolute ethyl alcohol and deionized water, obtains glue
Body shape aramid nano-fiber；
Wherein, the volume of washing absolute ethyl alcohol and the ratio of aramid fiber quality are 1mL:5mg~1mL:2mg, washing time
Number is 3~5 times；The mass ratio of the washing deionized water and aramid fiber is 10:1~5:1；
(5) aramid nano-fiber obtained in step (4) is scattered in deionized water or hydrophilic solvent under stirring
In, obtain homogeneous and transparent aramid nano-fiber water-dispersed；
Wherein, hydrophilic solvent is methanol, ethyl alcohol, propyl alcohol or isopropanol, and dispersion concentration is 0.5~5mg/mL；The stirring
Revolution is 500~2500rpm, 30~180min of mixing time.
A kind of preparation method of aramid fiber nanometer paper, including following preparation process：
(1) disperse：The aramid nano-fiber water-dispersed of above-mentioned preparation is scattered in deionized water, dispersion concentration 0.2
~5mg/mL；
(2) Top wire former：The aramid nano-fiber slurry that step (1) obtains forming of manufacturing paper with pulp on oblique net paper machine is obtained into virtue
Synthetic fibre nanometer paper, forming quality a concentration of 0.02%~0.06%；
(3) drying is squeezed：The aramid fiber nanometer paper that step (2) obtains is placed in squeezer to squeeze and dry, the squeezing item
Part is：0.2~1.0MPa of squeeze pressure squeezes 3~20min of time；The drying condition is：Drying temperature：90~110 DEG C,
5~15min of drying time.
The present invention is described in further detail with reference to embodiment：
Embodiment 1
A kind of preparation method of aramid nano-fiber water-dispersed of the present embodiment, specific preparation process are as follows：
(1) 1.0g p-aramid fibers yarn fibers, 1.5g potassium hydroxide (KOH) and 500ml dimethyl sulfoxide (DMSO)s (DMSO) are set
In container, under air-proof condition, is stirred 8 days at a temperature of 30 DEG C, obtain the aramid fiber nanometer being scattered under KOH/DMSO systems
Fiber dispersion；
(2) the aramid nano-fiber dispersion liquid being scattered under KOH/DMSO systems that will be obtained in step (1) is in rotating speed
Under 600rpm stirring actions, to its high-pressure injection deionized water, the mass ratio of deionized water and aramid fiber is 1:1, jet stream pressure
Power is 5MPa, and effluxvelocity 0.2ml/s obtains being scattered in KOH/DMSO/H2Aramid nano-fiber in O mixed systems；
(3) it is scattered in KOH/DMSO/H by what is obtained in step (2)2Aramid nano-fiber in O mixed systems passes through 200
Purpose nylon leaching film is filtered by vacuum, and obtains aramid nano-fiber；
(4) aramid nano-fiber obtained in step (3) is washed 3 repeatedly respectively by absolute ethyl alcohol and deionized water
Secondary, the volume of absolute ethyl alcohol needed for washing and the ratio of aramid fiber quality are 1ml every time:5mg, required deionized water are fine with aramid fiber
The mass ratio of dimension is 10:1, obtain colloidal aramid nano-fiber；
(5) by the aramid nano-fiber obtained in step (4) under the stirring action of 500rpm, stirring 150min is scattered in
In deionized water, dispersion concentration is controlled in 0.5mg/ml, obtains homogeneous and transparent aramid nano-fiber water-dispersed.
It is a kind of in the present embodiment to prepare aramid fiber nanometer paper using by aramid nano-fiber water-dispersed prepared by the above method
Method, including following preparation process：
(1) disperse：The aramid nano-fiber water-dispersed of above-mentioned preparation is scattered in deionized water, dispersion concentration is
0.2mg/ml；
(2) Top wire former：The aramid nano-fiber slurry that step (1) obtains forming of manufacturing paper with pulp on oblique net paper machine is obtained into virtue
Synthetic fibre nanometer paper, forming quality a concentration of 0.02%；
(3) drying is squeezed：The aramid fiber nanometer paper that step (2) obtains is placed in squeezer to squeeze and dry, squeezing condition is：
Squeeze pressure 0.2MPa squeezes time 20min；Drying condition is：Drying temperature：110 DEG C, drying time 5min.
Embodiment 2
A kind of preparation method of aramid nano-fiber water-dispersed of the present embodiment, specific preparation process are as follows：
(1) 1.0g p-aramid fibers chopped strand, 1.5g potassium hydroxide (KOH) and 500ml dimethyl sulfoxide (DMSO)s (DMSO) are set
In container, under air-proof condition, is stirred 7 days at a temperature of 40 DEG C, obtain the aramid fiber nanometer being scattered under KOH/DMSO systems
Fiber dispersion；
(2) the aramid nano-fiber dispersion liquid being scattered under KOH/DMSO systems that will be obtained in step (1) is in rotating speed
Under 1000rpm stirring actions, to its high-pressure injection deionized water, the mass ratio of deionized water and aramid fiber is 1.5:1, jet stream
Pressure is 7.5MPa, and effluxvelocity 0.3ml/s obtains being scattered in KOH/DMSO/H2Aramid fiber Nanowire in O mixed systems
Dimension；
(3) it is scattered in KOH/DMSO/H by what is obtained in step (2)2Aramid nano-fiber in O mixed systems passes through 250
Purpose nylon leaching film is filtered by vacuum, and obtains aramid nano-fiber；
(4) aramid nano-fiber obtained in step (3) is washed 4 repeatedly respectively by absolute ethyl alcohol and deionized water
Secondary, the volume of absolute ethyl alcohol needed for washing and the ratio of aramid fiber quality are 1ml every time:4mg, required deionized water are fine with aramid fiber
The mass ratio of dimension is 9:1, obtain colloidal aramid nano-fiber；
(5) by the aramid nano-fiber obtained in step (4) under the stirring action of 800rpm, stirring 120min is scattered in
In deionized water, dispersion concentration is controlled in 1.0mg/ml, obtains homogeneous and transparent aramid nano-fiber water-dispersed.
It is a kind of in the present embodiment to prepare aramid fiber nanometer paper using by aramid nano-fiber water-dispersed prepared by the above method
Method, including following preparation process：
(1) disperse：The aramid nano-fiber water-dispersed of above-mentioned preparation is scattered in deionized water, dispersion concentration is
0.4mg/ml；
(2) Top wire former：The aramid nano-fiber slurry that step (1) obtains forming of manufacturing paper with pulp on oblique net paper machine is obtained into virtue
Synthetic fibre nanometer paper, forming quality a concentration of 0.03%；
(3) drying is squeezed：The aramid fiber nanometer paper that step (2) obtains is placed in squeezer to squeeze and dry, squeezing condition is：
Squeeze pressure 0.4MPa squeezes time 15min；Drying condition is：Drying temperature：100 DEG C, drying time 10min.
Embodiment 3
A kind of preparation method of aramid nano-fiber water-dispersed of the present embodiment, specific preparation process are as follows：
(1) 1.0g para-aramid pulp fiber, 1.5g potassium hydroxide (KOH) and 500ml dimethyl sulfoxide (DMSO)s (DMSO) are set
In container, under air-proof condition, is stirred 5 days at a temperature of 50 DEG C, obtain the aramid fiber nanometer being scattered under KOH/DMSO systems
Fiber dispersion；
(2) the aramid nano-fiber dispersion liquid being scattered under KOH/DMSO systems that will be obtained in step (1) is in rotating speed
Under 1500rpm stirring actions, to its high-pressure injection deionized water, the mass ratio of deionized water and aramid fiber is 2:1, jet stream pressure
Power is 7MPa, and effluxvelocity 0.8ml/s obtains being scattered in KOH/DMSO/H2Aramid nano-fiber in O mixed systems；
(3) it is scattered in KOH/DMSO/H by what is obtained in step (2)2Aramid nano-fiber in O mixed systems passes through 300
Purpose nylon leaching film is filtered by vacuum, and obtains aramid nano-fiber；
(4) aramid nano-fiber obtained in step (3) is washed 3 repeatedly respectively by absolute ethyl alcohol and deionized water
Secondary, the volume of absolute ethyl alcohol needed for washing and the ratio of aramid fiber quality are 1ml every time:3.5mg, required deionized water and aramid fiber
The mass ratio of fiber is 8:1, obtain colloidal aramid nano-fiber；
(5) by the aramid nano-fiber obtained in step (4) under the stirring action of 1000rpm, stirring 90min is scattered in
In deionized water, dispersion concentration is controlled in 1.5mg/ml, obtains homogeneous and transparent aramid nano-fiber water-dispersed.
It is a kind of in the present embodiment to prepare aramid fiber nanometer paper using by aramid nano-fiber water-dispersed prepared by the above method
Method, including following preparation process：
(1) disperse：The aramid nano-fiber water-dispersed of above-mentioned preparation is scattered in deionized water, dispersion concentration is
0.8mg/ml；
(2) Top wire former：The aramid nano-fiber slurry that step (1) obtains forming of manufacturing paper with pulp on oblique net paper machine is obtained into virtue
Synthetic fibre nanometer paper, forming quality a concentration of 0.04%；
(3) drying is squeezed：The aramid fiber nanometer paper that step (2) obtains is placed in squeezer to squeeze and dry, squeezing condition is：
Squeeze pressure 0.8MPa squeezes time 10min；Drying condition is：Drying temperature：105 DEG C, drying time 8min.
Embodiment 4
A kind of preparation method of aramid nano-fiber water-dispersed of the present embodiment, specific preparation process are as follows：
(1) 1.0g p-aramid fibers fibrid, 1.5g potassium hydroxide (KOH) and 500ml dimethyl sulfoxide (DMSO)s (DMSO) are set
In container, under air-proof condition, is stirred 6 days at a temperature of 45 DEG C, obtain the aramid fiber nanometer being scattered under KOH/DMSO systems
Fiber dispersion；
(2) the aramid nano-fiber dispersion liquid being scattered under KOH/DMSO systems that will be obtained in step (1) is in rotating speed
Under 2000rpm stirring actions, to its high-pressure injection deionized water, the mass ratio of deionized water and aramid fiber is 2.5:1, jet stream
Pressure is 8MPa, and effluxvelocity 1.0ml/s obtains being scattered in KOH/DMSO/H2Aramid nano-fiber in O mixed systems；
(3) it is scattered in KOH/DMSO/H by what is obtained in step (2)2Aramid nano-fiber in O mixed systems passes through 400
Purpose nylon leaching film is filtered by vacuum, and obtains aramid nano-fiber；
(4) aramid nano-fiber obtained in step (3) is washed 5 repeatedly respectively by absolute ethyl alcohol and deionized water
Secondary, the volume of absolute ethyl alcohol needed for washing and the ratio of aramid fiber quality are 1ml every time:4mg, required deionized water are fine with aramid fiber
The mass ratio of dimension is 7:1, obtain colloidal aramid nano-fiber；
(5) by the aramid nano-fiber obtained in step (4) under the stirring action of 1300rpm, stirring 70min is scattered in
In deionized water, dispersion concentration is controlled in 2.0mg/ml, obtains homogeneous and transparent aramid nano-fiber water-dispersed.
It is a kind of in the present embodiment to prepare aramid fiber nanometer paper using by aramid nano-fiber water-dispersed prepared by the above method
Method, including following preparation process：
(1) disperse：The aramid nano-fiber water-dispersed of above-mentioned preparation is scattered in deionized water, dispersion concentration is
2.0mg/ml；
(2) Top wire former：The aramid nano-fiber slurry that step (1) obtains forming of manufacturing paper with pulp on oblique net paper machine is obtained into virtue
Synthetic fibre nanometer paper, forming quality a concentration of 0.05%；
(3) drying is squeezed：The aramid fiber nanometer paper that step (2) obtains is placed in squeezer to squeeze and dry, squeezing condition is：
Squeeze pressure 0.9MPa squeezes time 7min；Drying condition is：Drying temperature：100 DEG C, drying time 10min.
Embodiment 5
A kind of preparation method of aramid nano-fiber water-dispersed of the present embodiment, specific preparation process are as follows：
(1) 1.0g p-aramid fibers yarn fibers, 1.5g potassium hydroxide (KOH) and 500ml dimethyl sulfoxide (DMSO)s (DMSO) are set
In container, under air-proof condition, is stirred 7 days at a temperature of 40 DEG C, obtain the aramid fiber nanometer being scattered under KOH/DMSO systems
Fiber dispersion；
(2) the aramid nano-fiber dispersion liquid being scattered under KOH/DMSO systems that will be obtained in step (1) is in rotating speed
Under 2200rpm stirring actions, to its high-pressure injection deionized water, the mass ratio of deionized water and aramid fiber is 3:1, jet stream pressure
Power is 10MPa, and effluxvelocity 1.2ml/s obtains being scattered in KOH/DMSO/H2Aramid nano-fiber in O mixed systems；
(3) it is scattered in KOH/DMSO/H by what is obtained in step (2)2Aramid nano-fiber in O mixed systems passes through 400
Purpose nylon leaching film is filtered by vacuum, and obtains aramid nano-fiber；
(4) aramid nano-fiber obtained in step (3) is washed 4 repeatedly respectively by absolute ethyl alcohol and deionized water
Secondary, the volume of absolute ethyl alcohol needed for washing and the ratio of aramid fiber quality are 1ml every time:3.5mg, required deionized water and aramid fiber
The mass ratio of fiber is 6:1, obtain colloidal aramid nano-fiber；
(5) by the aramid nano-fiber obtained in step (4) under the stirring action of 1800rpm, stirring 50min is scattered in
In deionized water, dispersion concentration is controlled in 2.5mg/ml, obtains homogeneous and transparent aramid nano-fiber water-dispersed.
It is a kind of in the present embodiment to prepare aramid fiber nanometer paper using by aramid nano-fiber water-dispersed prepared by the above method
Method, including following preparation process：
(1) disperse：The aramid nano-fiber water-dispersed of above-mentioned preparation is scattered in deionized water, dispersion concentration is
3.0mg/ml；
(2) Top wire former：The aramid nano-fiber slurry that step (1) obtains forming of manufacturing paper with pulp on oblique net paper machine is obtained into virtue
Synthetic fibre nanometer paper, forming quality a concentration of 0.045%；
(3) drying is squeezed：The aramid fiber nanometer paper that step (2) obtains is placed in squeezer to squeeze and dry, squeezing condition is：
Squeeze pressure 0.7MPa squeezes time 9min；Drying condition is：Drying temperature：95 DEG C, drying time 12min.
Embodiment 6
A kind of preparation method of aramid nano-fiber water-dispersed of the present embodiment, specific preparation process are as follows：
(1) 1.0g p-aramid fibers chopped strand, 1.5g potassium hydroxide (KOH) and 500ml dimethyl sulfoxide (DMSO)s (DMSO) are set
In container, under air-proof condition, is stirred 7 days at a temperature of 30 DEG C, obtain the aramid fiber nanometer being scattered under KOH/DMSO systems
Fiber dispersion；
(2) the aramid nano-fiber dispersion liquid being scattered under KOH/DMSO systems that will be obtained in step (1) is in rotating speed
Under 2500rpm stirring actions, to its high-pressure injection deionized water, the mass ratio of deionized water and aramid fiber is 3.5:1, jet stream
Pressure is 12MPa, and effluxvelocity 1.5ml/s obtains being scattered in KOH/DMSO/H2Aramid nano-fiber in O mixed systems；
(3) it is scattered in KOH/DMSO/H by what is obtained in step (2)2Aramid nano-fiber in O mixed systems passes through 450
Purpose nylon leaching film is filtered by vacuum, and obtains aramid nano-fiber；
(4) aramid nano-fiber obtained in step (3) is washed 5 repeatedly respectively by absolute ethyl alcohol and deionized water
Secondary, the volume of absolute ethyl alcohol needed for washing and the ratio of aramid fiber quality are 1ml every time:2.5mg, required deionized water and aramid fiber
The mass ratio of fiber is 7:1, obtain colloidal aramid nano-fiber；
(5) by the aramid nano-fiber obtained in step (4) under the stirring action of 2000rpm, stirring 45min is scattered in
In deionized water, dispersion concentration is controlled in 3.0mg/ml, obtains homogeneous and transparent aramid nano-fiber water-dispersed.
It is a kind of in the present embodiment to prepare aramid fiber nanometer paper using by aramid nano-fiber water-dispersed prepared by the above method
Method, including following preparation process：
(1) disperse：The aramid nano-fiber water-dispersed of above-mentioned preparation is scattered in deionized water, dispersion concentration is
3.5mg/ml；
(2) Top wire former：The aramid nano-fiber slurry that step (1) obtains forming of manufacturing paper with pulp on oblique net paper machine is obtained into virtue
Synthetic fibre nanometer paper, forming quality a concentration of 0.055%；
(3) drying is squeezed：The aramid fiber nanometer paper that step (2) obtains is placed in squeezer to squeeze and dry, squeezing condition is：
Squeeze pressure 0.9MPa squeezes time 7min；Drying condition is：Drying temperature：100 DEG C, drying time 8min.
Embodiment 7
A kind of preparation method of aramid nano-fiber water-dispersed of the present embodiment, specific preparation process are as follows：
(1) 1.0g para-aramid pulp fiber, 1.5g potassium hydroxide (KOH) and 500ml dimethyl sulfoxide (DMSO)s (DMSO) are set
In container, under air-proof condition, is stirred 7 days at a temperature of 40 DEG C, obtain the aramid fiber nanometer being scattered under KOH/DMSO systems
Fiber dispersion；
(2) the aramid nano-fiber dispersion liquid being scattered under KOH/DMSO systems that will be obtained in step (1) is in rotating speed
Under 2800rpm stirring actions, to its high-pressure injection deionized water, the mass ratio of deionized water and aramid fiber is 4:1, jet stream pressure
Power is 13MPa, and effluxvelocity 1.7ml/s obtains being scattered in KOH/DMSO/H2Aramid nano-fiber in O mixed systems；
(3) it is scattered in KOH/DMSO/H by what is obtained in step (2)2Aramid nano-fiber in O mixed systems passes through 500
Purpose nylon leaching film is filtered by vacuum, and obtains aramid nano-fiber；
(4) aramid nano-fiber obtained in step (3) is washed 4 repeatedly respectively by absolute ethyl alcohol and deionized water
Secondary, the volume of absolute ethyl alcohol needed for washing and the ratio of aramid fiber quality are 1ml every time:2mg, required deionized water are fine with aramid fiber
The mass ratio of dimension is 6:1, obtain colloidal aramid nano-fiber；
(5) by the aramid nano-fiber obtained in step (4) under the stirring action of 2300rpm, stirring 40min is scattered in
In deionized water, dispersion concentration is controlled in 4.0mg/ml, obtains homogeneous and transparent aramid nano-fiber water-dispersed.
It is a kind of in the present embodiment to prepare aramid fiber nanometer paper using by aramid nano-fiber water-dispersed prepared by the above method
Method, including following preparation process：
(1) disperse：The aramid nano-fiber water-dispersed of above-mentioned preparation is scattered in deionized water, dispersion concentration 4mg/
ml；
(2) Top wire former：The aramid nano-fiber slurry that step (1) obtains forming of manufacturing paper with pulp on oblique net paper machine is obtained into virtue
Synthetic fibre nanometer paper, forming quality a concentration of 0.06%；
(3) drying is squeezed：The aramid fiber nanometer paper that step (2) obtains is placed in squeezer to squeeze and dry, squeezing condition is：
Squeeze pressure 0.8MPa squeezes time 8min；Drying condition is：Drying temperature：95 DEG C, drying time 12min.
Embodiment 8
A kind of preparation method of aramid nano-fiber water-dispersed of the present embodiment, specific preparation process are as follows：
(1) 1.0g p-aramid fibers fibrid, 1.5g potassium hydroxide (KOH) and 500ml dimethyl sulfoxide (DMSO)s (DMSO) are set
In container, under air-proof condition, is stirred 7 days at a temperature of 50 DEG C, obtain the aramid fiber nanometer being scattered under KOH/DMSO systems
Fiber dispersion；
(2) the aramid nano-fiber dispersion liquid being scattered under KOH/DMSO systems that will be obtained in step (1) is in rotating speed
Under 3000rpm stirring actions, to its high-pressure injection deionized water, the mass ratio of deionized water and aramid fiber is 5:1, jet stream pressure
Power is 15MPa, and effluxvelocity 2ml/s obtains being scattered in KOH/DMSO/H2Aramid nano-fiber in O mixed systems；
(3) it is scattered in KOH/DMSO/H by what is obtained in step (2)2Aramid nano-fiber in O mixed systems passes through 500
Purpose nylon leaching film is filtered by vacuum, and obtains aramid nano-fiber；
(4) aramid nano-fiber obtained in step (3) is washed 5 repeatedly respectively by absolute ethyl alcohol and deionized water
Secondary, the volume of absolute ethyl alcohol needed for washing and the ratio of aramid fiber quality are 1ml every time:2mg, required deionized water are fine with aramid fiber
The mass ratio of dimension is 5:1, obtain colloidal aramid nano-fiber；
(5) by the aramid nano-fiber obtained in step (4) under the stirring action of 2500rpm, stirring 30min is scattered in
In deionized water, dispersion concentration is controlled in 5.0mg/ml, obtains homogeneous and transparent aramid nano-fiber water-dispersed.
It is a kind of in the present embodiment to prepare aramid fiber nanometer paper using by aramid nano-fiber water-dispersed prepared by the above method
Method, including following preparation process：
(1) disperse：The aramid nano-fiber water-dispersed of above-mentioned preparation is scattered in deionized water, dispersion concentration 5mg/
ml；
(2) Top wire former：The aramid nano-fiber slurry that step (1) obtains forming of manufacturing paper with pulp on oblique net paper machine is obtained into virtue
Synthetic fibre nanometer paper, forming quality a concentration of 0.06%；
(3) drying is squeezed：The aramid fiber nanometer paper that step (2) obtains is placed in squeezer to squeeze and dry, squeezing condition is：
Squeeze pressure 1.0MPa squeezes time 5min；Drying condition is：Drying temperature：90 DEG C, drying time 15min.
Characterization is detected to aramid nano-fiber water-dispersed made from the embodiment of the present invention 6, a diameter of 20.5 ±
3.4nm, crystallinity 82%, TG10%532℃.The aramid fiber nanometer paper prepared to the method for the present invention is detected characterization, and part refers to
Mark is respectively：1, quantitative：40.0m2/g；2, tensile strength：97.0MPa；3, tearing strength：204.21mN；4, compressive resistance：
86.3kV/mm；5、TG10%：535.6℃.Aramid nano-fiber prepared by the present invention, can be completely in aqueous phase system or hydrophily
Uniformly and stably disperse in solvent, and aramid nano-fiber diameter is small, draw ratio is big, high surface activity, Good Heat-resistance.This
Aramid nano-fiber water-dispersed prepared by invention method described above is aramid fiber nanometer paper prepared by raw material, good with forming evenness,
The advantages that paper structure densification, mechanical strength and compressive resistance are had excellent performance, can be used as High Performance Insulation material and is widely used in
High-end electric insulation field.
Claims (9)
1. a kind of preparation method of aramid nano-fiber water-dispersed, which is characterized in that include the following steps：
(1) para-aramid fiber, potassium hydroxide, dimethyl sulfoxide (DMSO) are placed in container, are dispersed with stirring, obtain being scattered in KOH/
Aramid nano-fiber dispersion liquid under DMSO system；
(2) the aramid nano-fiber dispersion liquid being scattered under KOH/DMSO systems that will be obtained in step (1), in stirring action
Under, to its high-pressure injection deionized water, obtain being scattered in KOH/DMSO/H2Aramid nano-fiber in O mixed systems；
(3) it is scattered in KOH/DMSO/H by what is obtained in step (2)2Aramid nano-fiber in O mixed systems is taken out by vacuum
Filter, obtains aramid nano-fiber；
(4) aramid nano-fiber obtained in step (3) is washed repeatedly by absolute ethyl alcohol and deionized water, obtains colloidal
Aramid nano-fiber；
(5) the colloidal aramid nano-fiber obtained in step (4) is scattered in deionized water or hydrophilic molten under stirring
In agent, aramid nano-fiber water-dispersed is obtained.
2. a kind of preparation method of aramid nano-fiber water-dispersed according to claim 1, which is characterized in that step (1)
Middle para-aramid fiber, potassium hydroxide and dimethyl sulfoxide (DMSO) ratio are 1g：1.5g：500ml, the para-aramid fiber are pair
One kind in position aramid yarn fiber, p-aramid fiber chopped strand, para-aramid pulp fiber and p-aramid fiber fibrid.
3. a kind of preparation method of aramid nano-fiber water-dispersed according to claim 1, which is characterized in that step (2)
Described in high-pressure injection be utilize stainless steel high-pressure spray pump, jet pressure be 5~15MPa, effluxvelocity be 0.2~
2.0mL/s；The mass ratio of jet stream deionized water and para-aramid fiber is 1:1~5:1.
4. a kind of preparation method of aramid nano-fiber water-dispersed according to claim 1, which is characterized in that step (3)
The middle filter membrane used that is filtered by vacuum is 200~500 mesh nylon leaching film.
5. a kind of preparation method of aramid nano-fiber water-dispersed according to claim 1, which is characterized in that step (4)
The volume of middle washing absolute ethyl alcohol and the ratio of aramid fiber quality are 1mL:5mg~1mL:2mg；The washing deionized water
Mass ratio with aramid fiber is 10:1~5:1.
6. a kind of preparation method of aramid nano-fiber water-dispersed according to claim 1, which is characterized in that step (5)
Middle hydrophilic solvent is methanol, ethyl alcohol, propyl alcohol or isopropanol, and colloidal aramid nano-fiber is in deionized water or hydrophilic solvent
Dispersion concentration be 0.5~5mg/mL.
7. a kind of preparation method of aramid nano-fiber water-dispersed according to claim 1, which is characterized in that step (1)
Middle stirring refers to being stirred 5~8 days at a temperature of 30~50 DEG C under air-proof condition；In step (2) speed of agitator be 600~
3000rpm；Agitation revolution is 500~2500rpm, 30~180min of mixing time in step (5).
8. a kind of aramid nano-fiber water-dispersed prepared using any one of claim 1-7 methods prepares the side of aramid fiber nanometer paper
Method, which is characterized in that include the following steps：
(1) disperse：Aramid nano-fiber water-dispersed is scattered in deionized water and obtains aramid nano-fiber slurry, dispersion concentration
For 0.2~5mg/mL；
(2) Top wire former：The aramid nano-fiber slurry that step (1) obtains forming of manufacturing paper with pulp on oblique net paper machine is obtained aramid fiber and receives
Rice paper l Water Paper, forming quality a concentration of 0.02%~0.06%；
(3) drying is squeezed：The aramid fiber nanometer paper l Water Paper that step (2) obtains is placed in squeezer to squeeze and be dried to obtain aramid fiber nanometer
Paper.
9. the preparation method of aramid fiber nanometer paper according to claim 8, which is characterized in that step squeezes item described in (3)
Part is：0.2~1.0MPa of squeeze pressure squeezes 3~20min of time；The drying condition is：Drying temperature：90~110 DEG C,
5~15min of drying time.
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| CN113737306A (en) * | 2021-09-07 | 2021-12-03 | 华南理工大学 | Aramid fiber micro-nano fiber with dendritic structure prepared by double-jet method and application thereof |
| CN113862816A (en) * | 2021-10-12 | 2021-12-31 | 天津科技大学 | Preparation method of short rod-shaped aramid nanofiber, aramid nanofiber and application |
| CN113862816B (en) * | 2021-10-12 | 2023-09-22 | 天津科技大学 | Preparation method of short-rod-shaped aramid nanofiber and application |
| CN113914130A (en) * | 2021-10-13 | 2022-01-11 | 浙江理工大学绍兴柯桥研究院有限公司 | Superfine nano aramid fiber and controllable preparation method of paper material thereof |
| CN113914130B (en) * | 2021-10-13 | 2023-03-14 | 浙江理工大学绍兴柯桥研究院有限公司 | Superfine nano aramid fiber and controllable preparation method of paper material thereof |
| CN115928242A (en) * | 2022-11-24 | 2023-04-07 | 清华大学 | Preparation method of superfine para-aramid nano-fiber and dispersion liquid thereof |
| CN115928242B (en) * | 2022-11-24 | 2023-10-20 | 清华大学 | Preparation method of superfine para-aramid nanofiber and dispersion liquid thereof |
| CN116024840A (en) * | 2022-12-13 | 2023-04-28 | 国网湖南省电力有限公司 | Carbon fluoride nanotube/aramid nanofiber composite insulating paper and preparation method thereof |
| CN116218212A (en) * | 2023-03-31 | 2023-06-06 | 陕西科技大学 | Aramid nanofiber wave-absorbing honeycomb material and preparation method thereof |
| CN116876253A (en) * | 2023-06-14 | 2023-10-13 | 哈尔滨工程大学 | Controllable preparation method of multifunctional aramid nanofiber wave-absorbing composite membrane |
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