CN108285540B - Preparation method of water-dispersible aramid nanofiber and aramid nano paper - Google Patents
Preparation method of water-dispersible aramid nanofiber and aramid nano paper Download PDFInfo
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- 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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- C08J2377/00—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
The invention discloses a preparation method of water dispersible aramid nano-fiber and aramid nano-paper, the aramid nano-fiber prepared by the invention can be completely dispersed in a water phase system or a hydrophilic solvent uniformly and stably, the preparation process flow of the method is simple, the short-flow preparation is realized, the control is easy, the method is suitable for industrial production, and the problems that the existing aramid nano-fiber can only be uniformly dispersed in a strong base/DMSO system, can not be uniformly and stably dispersed in the water phase system, can not be stored for a long time and the like are solved; greatly expands the blending and enhancing application of the aramid nano-fiber, the water-soluble polymer and the hydrophilic material. The aramid nano paper prepared by using the water dispersible aramid nano fiber prepared by the method as the raw material has the advantages of good forming uniformity, compact paper structure, excellent mechanical strength and compressive strength performance and the like, and can be widely applied to the high-end electrical insulation field as a high-performance insulating material.
Description
Technical Field
The invention belongs to the field of polymer nano materials and papermaking, and particularly relates to a preparation method of water-dispersible aramid nano fibers and aramid nano paper.
Background
Para-aramid fiber (PPTA) is a high-performance synthetic fiber with high strength, high modulus, insulating property and excellent high-temperature resistance, is an ideal raw material for protective and reinforcing materials, and is widely applied to the fields of aerospace, national defense, electronic communication, petrochemical industry and the like. The high-strength high-temperature-resistant characteristic of the para-aramid fiber is derived from a rigid chain structure formed by pi-pi conjugation in a molecular chain, a compact and ordered two-dimensional network structure formed by hydrogen bonds between molecular chains and van der Waals acting force and the like. However, due to the structural characteristics, the aramid fiber has the defects of smooth surface, few active groups, strong chemical inertness and the like, so that the interface bonding force between the aramid fiber and the matrix such as resin is poor, and the application of the aramid fiber in high-value-added fields such as high-performance composite reinforced materials, nano materials, filter materials, biological medicines and the like is limited.
Aramid Nanofibers (ANFs) serving as polymer Nanofibers with excellent performance emerging in recent years are similar to inorganic nano reinforcing materials (such as nano particles, nano wires, nano tubes and nano sheets) which are most applied in the field of materials, have unique nanoscale structures, large length-diameter ratio and specific surface area, and simultaneously retain excellent mechanical properties and temperature resistance of Aramid macroscopic fibers, bring mechanical properties, electrical properties and optical properties which cannot be realized by conventional chemical fibers to the Aramid Nanofibers, enable the Aramid Nanofibers to become novel building units for building macroscopic composite materials, play an important role in interface reinforcement, and have great application prospects in the fields of composite materials, biology, medicine, electronics, energy and the like.
Aramid nanofibers were first prepared by the chemical alkali dissolution method taught by professor of the U.S. Nicholas A.Kotov task group (Yang M, Cao K, Sui L, et al.dispersions of aramid nanofibers: and nanoscaled fibers Block [ J ]. Acs Nano,2011,5(9): 6945-54.). Aramid fiber is mixed with strong base (KOH) and Dimethyl sulfoxide (DMSO) and then is continuously stirred for 7-10 days at room temperature, and the ANFs/DMSO dispersion liquid with stable homogeneous dispersion is obtained. The KOH/DMSO strong base system can directionally and effectively destroy the cross-linking effect of hydrogen bonds between macroscopic aramid fiber molecular chains, simultaneously break N-H bonds on amido bonds to be deprotonated to form nitrogen anions, and the molecular chains with negative charges are dispersed and stably exist under the action of electrostatic repulsion, pi-pi conjugated acting force generated by benzene rings and the amido bonds and intermolecular van der Waals force.
However, the aramid nanofibers prepared by the method can only exist in a strong alkali/DMSO system, when the dispersion liquid contains a proton donor (for example, when the dispersion liquid becomes neutral or weak alkali), nitrogen anions acquire hydrogen atoms again, hydrogen bonds among the aramid nanofibers are formed again, and the fibers are condensed again. Particularly, when the dispersion liquid is water, a large amount of aramid nano-fibers can be subjected to protonation reduction, and easily generate aggregation to form a film-shaped or aggregated precipitate; in addition, because DMSO in the ANFs/DMSO system is easy to absorb water in humid air and is easy to be protonated and reduced to form a film-shaped or aggregated precipitate, the prepared aramid fiber nano solution cannot be stored for a long time. Therefore, the aramid nano-fiber solution prepared by the method has the problems that the solution can only be dispersed in a strong alkali/DMSO system, cannot be uniformly and stably dispersed in a water phase system, cannot be stored for a long time and the like, and the application of the solution in water-soluble polymers and hydrophilic materials is greatly limited, so that the aramid nano-fiber with excellent performance cannot realize a remarkable enhancement effect, and the application field of the aramid nano-fiber solution is limited.
In order to solve the problem, at present, a main solution is to react an active functional group organic small molecule (such as bromopropyne, chloropropyne, 5-chloro-1-pentyne, 1-bromo-2-butyne, and the like) capable of performing an affinity reaction with a nitrogen anion with an aramid nanofiber to obtain an aramid nanofiber with an active functional group, then react the aramid nanofiber with an active water-soluble high molecular compound [ such as polyethylene glycol monomethyl ether azide (m-PEG-N3), polyethylene oxide azide (PEO-N3), and polyacrylic acid azide (PA-N3) ] to obtain an aramid nanofiber with a water-soluble functional group, and then freeze-dry the aramid nanofiber to remove a solvent and disperse the aramid nanofiber in an aqueous solution to obtain a water-dispersed aramid nanofiber (patent No. 201410833596.3). However, the solution proposed in this patent also presents the following problems: firstly, the surface of the aramid nano fiber is reacted to be provided with water-soluble small molecules or functional groups, so that the strength, the modulus and the heat resistance of the aramid nano fiber are reduced; secondly, the multi-step reaction method needs a catalyst and reacts under the anaerobic condition, and the preparation process and the process are complex; thirdly, freeze drying is needed in the preparation process, and the energy consumption is large, which is not beneficial to industrial production.
Disclosure of Invention
The invention aims to provide a preparation method of water-dispersible aramid nano-fiber and aramid nano-paper, which overcomes the defects in the prior art and solves the problems that the existing aramid nano-fiber can only be uniformly dispersed in a strong alkali/DMSO system, can not be uniformly and stably dispersed in a water phase system, can not be stored for a long time and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of water-dispersible aramid nano-fibers comprises the following steps:
(1) placing para-aramid fiber, potassium hydroxide and dimethyl sulfoxide into a container, and stirring and dispersing to obtain an aramid nanofiber dispersion liquid dispersed in a KOH/DMSO system;
(2) injecting deionized water into the aramid nano-fiber dispersion liquid dispersed in a KOH/DMSO system obtained in the step (1) under the stirring action at high pressure to obtain the aramid nano-fiber dispersion liquid dispersed in KOH/DMSO/H2Aramid nanofibers in an O mixing system;
(3) dispersing the obtained product in the step (2) in KOH/DMSO/H2Carrying out vacuum filtration on the aramid nano-fiber in the O mixed system to obtain the aramid nano-fiber;
(4) repeatedly washing the aramid nano-fiber obtained in the step (3) by absolute ethyl alcohol and deionized water to obtain colloidal aramid nano-fiber;
(5) and (4) dispersing the colloidal aramid nano-fiber obtained in the step (4) in deionized water or a hydrophilic solvent under the stirring action to obtain the water-dispersed aramid nano-fiber.
Further, in the step (1), the proportion of the para-aramid fiber, the potassium hydroxide and the dimethyl sulfoxide is 1 g: 1.5 g: 500ml, the para-aramid fiber is one of para-aramid yarn fiber, para-aramid chopped fiber, para-aramid pulp fiber and para-aramid fibrid.
Further, the high-pressure injection in the step (2) is performed by using a stainless steel high-pressure jet pump, the jet pressure is 5-15 MPa, and the jet speed is 0.2-2.0 mL/s; the mass ratio of the jet flow deionized water to the para-aramid fiber is 1: 1-5: 1.
Further, the filter membrane adopted in the vacuum filtration in the step (3) is a nylon filter membrane of 200-500 meshes.
Further, the ratio of the volume of the absolute ethyl alcohol for washing in the step (4) to the mass of the aramid fiber is 1mL:5 mg-1 mL:2 mg; the mass ratio of the deionized water for washing to the aramid fiber is 10: 1-5: 1.
Further, the hydrophilic solvent in the step (5) is methanol, ethanol, propanol or isopropanol, and the dispersion concentration of the colloidal aramid nanofiber in deionized water or the hydrophilic solvent is 0.5-5 mg/mL.
Further, the stirring in the step (1) is to stir for 5-8 days at the temperature of 30-50 ℃ under a sealed condition; in the step (2), the stirring speed is 600-3000 rpm; in the step (5), the stirring revolution is 500-2500 rpm, and the stirring time is 30-180 min.
A method for preparing aramid nano-paper by adopting water dispersible aramid nano-fibers comprises the following steps:
(1) dispersing: dispersing water-dispersed aramid nano-fibers in deionized water to obtain aramid nano-fiber slurry, wherein the dispersion concentration is 0.2-5 mg/mL;
(2) and (3) net surfing and forming: making and forming the aramid nano-fiber pulp obtained in the step (1) on an inclined wire paper machine to obtain aramid nano-paper wet paper, wherein the forming mass concentration is 0.02-0.06%;
(3) squeezing and drying: and (3) placing the aramid fiber nano paper wet paper obtained in the step (2) in a squeezer to be squeezed and dried to obtain aramid fiber nano paper base paper.
Further, the pressing conditions in the step (3) are as follows: the squeezing pressure is 0.2-1.0 MPa, and the squeezing time is 3-20 min; the drying conditions are as follows: drying temperature: and drying for 5-15 min at 90-110 ℃.
Compared with the prior art, the invention has the following beneficial technical effects:
the water dispersible aramid nano-fiber prepared by the invention solves the problems that the existing aramid nano-fiber can only be uniformly dispersed in a strong alkali/DMSO system, can not be uniformly and stably dispersed in a water phase system, can not be stored for a long time and the like; solves the problems that the prior art has reduced strength, modulus and heat resistance caused by the reaction of water-soluble micromolecules or functional groups, and the prior preparation technology has rigorous reaction conditions, complex preparation process and the like.
The water-dispersible aramid nano-fiber prepared by the method can be uniformly and stably dispersed in a water phase system or a hydrophilic solvent, and the aramid nano-fiber has the advantages of good dimensional stability, high film-forming strength, excellent heat resistance and simple preparation process flow, realizes short-flow preparation and easy control, is suitable for industrial production, and greatly expands the blending and enhancing application of the aramid nano-fiber, a water-soluble polymer and a hydrophilic material.
The water dispersible aramid nano-fiber prepared by the method can completely form uniform and stable suspension in a water phase system, so the aramid nano-paper prepared by using the water dispersible aramid nano-fiber prepared by the method as a raw material has the advantages of good forming uniformity, compact paper structure, excellent mechanical strength and compressive strength performance and the like, does not need a hot pressing treatment process required in the production process of the traditional aramid paper, has simple preparation flow and low energy consumption, can be widely applied to the field of electrical insulation as a high-performance insulating material, realizes small volume and large capacity of electrical insulation equipment, and promotes product upgrading and technical progress in the electrical insulation industry.
The water dispersible aramid nano fiber with excellent performance and the aramid nano paper prepared by using the water dispersible aramid nano fiber with excellent performance, which are researched and developed by a new process and a new method, solve the technical problems and the product defects in the prior art, have strong innovation, excellent product performance and wide application prospect, and have certain practical significance for promoting the development of high and new technology industries such as composite materials, promoting the upgrading and updating of the traditional industry, promoting the product grade and promoting the development of related industries and industries.
Drawings
FIG. 1 is a diagram showing the binding effect of the structural formula of PPTA molecule and hydrogen bonds between molecules;
fig. 2 is an SEM image of the surface of the aramid nanopaper obtained in example 6 of the present invention.
Detailed Description
Embodiments of the invention are described in further detail below:
a preparation method of water-dispersible aramid nano-fibers comprises the following preparation steps:
(1) placing para-aramid fiber, potassium hydroxide (KOH) and dimethyl sulfoxide (DMSO) in a container, and stirring and dispersing to obtain an aramid nanofiber dispersion liquid dispersed in a KOH/DMSO system;
wherein, the proportion of the para-aramid fiber, KOH and DMSO is 1 g: 1.5 g: 500 mL; the stirring is carried out for 5-8 days at the temperature of 30-50 ℃ under the sealed condition; the para-aramid fiber is one of para-aramid yarn fiber, para-aramid chopped fiber, para-aramid pulp fiber and para-aramid fibrid;
(2) injecting deionized water into the aramid nano-fiber dispersion liquid dispersed in a KOH/DMSO system obtained in the step (1) under the stirring action at high pressure to obtain the aramid nano-fiber dispersion liquid dispersed in KOH/DMSO/H2Aramid nanofibers in an O mixing system;
wherein the stirring action is high-shear stirring, and the stirring speed is 600-3000 rpm; the high-pressure injection is performed by using a stainless steel high-pressure jet pump, the jet pressure is 5-15 MPa, and the jet speed is 0.2-2.0 mL/s; the mass ratio of the jet flow deionized water to the aramid fiber is 1: 1-5: 1;
(3) dispersing the obtained product in the step (2) in KOH/DMSO/H2Carrying out vacuum filtration on the aramid nano-fiber in the O mixed system to obtain the aramid nano-fiber;
wherein the filter membrane adopted by vacuum filtration is a nylon filter membrane of 200-500 meshes;
(4) repeatedly washing the aramid nano-fiber obtained in the step (3) by absolute ethyl alcohol and deionized water to obtain colloidal aramid nano-fiber;
wherein the ratio of the volume of the absolute ethyl alcohol for washing to the mass of the aramid fiber is 1mL to 5 mg-1 mL to 2mg, and the washing times are 3-5 times; the mass ratio of the washing deionized water to the aramid fiber is 10: 1-5: 1;
(5) dispersing the aramid nano-fiber obtained in the step (4) in deionized water or a hydrophilic solvent under the stirring action to obtain uniform and transparent water-dispersed aramid nano-fiber;
wherein the hydrophilic solvent is methanol, ethanol, propanol or isopropanol, and the dispersion concentration is 0.5-5 mg/mL; the stirring revolution is 500-2500 rpm, and the stirring time is 30-180 min.
A preparation method of aramid nano paper comprises the following preparation steps:
(1) dispersing: dispersing the prepared water-dispersible aramid nano-fiber in deionized water, wherein the dispersion concentration is 0.2-5 mg/mL;
(2) and (3) net surfing and forming: making and forming the aramid nano-fiber pulp obtained in the step (1) on an inclined wire paper machine to obtain aramid nano-paper, wherein the forming mass concentration is 0.02-0.06%;
(3) squeezing and drying: placing the aramid nano paper obtained in the step (2) in a presser to press and dry, wherein the pressing conditions are as follows: the squeezing pressure is 0.2-1.0 MPa, and the squeezing time is 3-20 min; the drying conditions are as follows: drying temperature: and drying for 5-15 min at 90-110 ℃.
The present invention is described in further detail below with reference to examples:
example 1
The preparation method of the water-dispersible aramid nanofiber provided by the embodiment comprises the following specific preparation steps:
(1) placing 1.0g of para-aramid yarn fiber, 1.5g of potassium hydroxide (KOH) and 500ml of dimethyl sulfoxide (DMSO) in a container, and stirring for 8 days at the temperature of 30 ℃ under a sealed condition to obtain an aramid nanofiber dispersion liquid dispersed in a KOH/DMSO system;
(2) injecting deionized water into the aramid nano-fiber dispersion liquid dispersed in a KOH/DMSO system obtained in the step (1) under the stirring action of the rotation speed of 600rpm, wherein the mass ratio of the deionized water to the aramid fiber is 1:1, the jet pressure is 5MPa, and the jet speed is 0.2ml/s, so as to obtain the aramid nano-fiber dispersion liquid dispersed in the KOH/DMSO/H system2Aramid nanofibers in an O mixing system;
(3) dispersing the obtained product in the step (2) in KOH/DMSO/H2Carrying out vacuum filtration on the aramid nano-fiber in the O mixed system through a nylon filter membrane of 200 meshes to obtain the aramid nano-fiber;
(4) respectively and repeatedly washing the aramid nano-fiber obtained in the step (3) for 3 times by using absolute ethyl alcohol and deionized water, wherein the ratio of the volume of the absolute ethyl alcohol to the mass of the aramid fiber required in each washing is 1ml:5mg, and the mass ratio of the deionized water to the aramid fiber is 10:1, so as to obtain colloidal aramid nano-fiber;
(5) and (4) stirring the aramid nano-fiber obtained in the step (4) for 150min under the stirring action of 500rpm, and dispersing in deionized water, wherein the dispersion concentration is controlled to be 0.5mg/ml, so as to obtain uniform and transparent water-dispersed aramid nano-fiber.
In this embodiment, a method for preparing aramid nanopaper by using the water-dispersible aramid nanofiber prepared by the above method includes the following steps:
(1) dispersing: dispersing the prepared water-dispersed aramid nano-fiber in deionized water, wherein the dispersion concentration is 0.2 mg/ml;
(2) and (3) net surfing and forming: making and forming the aramid nano-fiber pulp obtained in the step (1) on an inclined wire paper machine to obtain aramid nano-paper, wherein the forming mass concentration is 0.02%;
(3) squeezing and drying: placing the aramid nano paper obtained in the step (2) in a squeezer to squeeze and dry, wherein the squeezing conditions are as follows: the squeezing pressure is 0.2MPa, and the squeezing time is 20 min; the drying conditions were: drying temperature: drying at 110 deg.C for 5 min.
Example 2
The preparation method of the water-dispersible aramid nanofiber provided by the embodiment comprises the following specific preparation steps:
(1) placing 1.0g of para-aramid chopped fiber, 1.5g of potassium hydroxide (KOH) and 500ml of dimethyl sulfoxide (DMSO) in a container, and stirring for 7 days at 40 ℃ under a sealed condition to obtain an aramid nano-fiber dispersion liquid dispersed in a KOH/DMSO system;
(2) injecting deionized water into the aramid nano-fiber dispersion liquid dispersed in a KOH/DMSO system obtained in the step (1) under the stirring action of the rotation speed of 1000rpm, wherein the mass ratio of the deionized water to the aramid fiber is 1.5:1, the jet pressure is 7.5MPa, and the jet speed is 0.3ml/s, so as to obtain the aramid nano-fiber dispersion liquid dispersed in the KOH/DMSO/H system2Aramid nanofibers in an O mixing system;
(3) dispersing the obtained product in the step (2) in KOH/DMSO/H2Carrying out vacuum filtration on the aramid nano-fiber in the O mixed system through a 250-mesh nylon filter membrane to obtain the aramid nano-fiber;
(4) respectively and repeatedly washing the aramid nano-fiber obtained in the step (3) for 4 times by using absolute ethyl alcohol and deionized water, wherein the ratio of the volume of the absolute ethyl alcohol to the mass of the aramid fiber required in each washing is 1ml:4mg, and the mass ratio of the deionized water to the aramid fiber is 9:1, so as to obtain colloidal aramid nano-fiber;
(5) and (4) stirring the aramid nano-fiber obtained in the step (4) for 120min under the stirring action of 800rpm, and dispersing in deionized water, wherein the dispersion concentration is controlled to be 1.0mg/ml, so as to obtain uniform and transparent water-dispersed aramid nano-fiber.
In this embodiment, a method for preparing aramid nanopaper by using the water-dispersible aramid nanofiber prepared by the above method includes the following steps:
(1) dispersing: dispersing the prepared water-dispersed aramid nano-fiber in deionized water, wherein the dispersion concentration is 0.4 mg/ml;
(2) and (3) net surfing and forming: making and forming the aramid nano-fiber pulp obtained in the step (1) on an inclined wire paper machine to obtain aramid nano-paper, wherein the forming mass concentration is 0.03%;
(3) squeezing and drying: placing the aramid nano paper obtained in the step (2) in a squeezer to squeeze and dry, wherein the squeezing conditions are as follows: the squeezing pressure is 0.4MPa, and the squeezing time is 15 min; the drying conditions were: drying temperature: drying at 100 deg.C for 10 min.
Example 3
The preparation method of the water-dispersible aramid nanofiber provided by the embodiment comprises the following specific preparation steps:
(1) placing 1.0g of para-aramid pulp fiber, 1.5g of potassium hydroxide (KOH) and 500ml of dimethyl sulfoxide (DMSO) in a container, and stirring for 5 days at 50 ℃ under a sealed condition to obtain an aramid nanofiber dispersion liquid dispersed in a KOH/DMSO system;
(2) injecting deionized water into the aramid nano-fiber dispersion liquid dispersed in a KOH/DMSO system obtained in the step (1) under the stirring action of 1500rpm, wherein the mass ratio of the deionized water to the aramid fiber is 2:1, the jet pressure is 7MPa, and the jet speed is 0.8ml/s, so as to obtain the aramid nano-fiber dispersion liquid dispersed in a KOH/DMSO/H system2Aramid nanofibers in an O mixing system;
(3) dispersing the dispersion obtained in step (2) in KOH/DMSO/H2Carrying out vacuum filtration on the aramid nano-fiber in the O mixed system through a 300-mesh nylon filter membrane to obtain the aramid nano-fiber;
(4) respectively and repeatedly washing the aramid nano-fiber obtained in the step (3) for 3 times by using absolute ethyl alcohol and deionized water, wherein the ratio of the volume of the absolute ethyl alcohol to the mass of the aramid fiber required in each washing is 1ml:3.5mg, and the mass ratio of the deionized water to the aramid fiber is 8:1, so as to obtain a colloidal aramid nano-fiber;
(5) and (4) stirring the aramid nano-fiber obtained in the step (4) for 90min under the stirring action of 1000rpm, and dispersing in deionized water, wherein the dispersion concentration is controlled to be 1.5mg/ml, so as to obtain uniform and transparent water-dispersed aramid nano-fiber.
In this embodiment, a method for preparing aramid nanopaper by using the water-dispersible aramid nanofiber prepared by the above method includes the following steps:
(1) dispersing: dispersing the prepared water-dispersed aramid nano-fiber in deionized water, wherein the dispersion concentration is 0.8 mg/ml;
(2) and (3) net surfing and forming: making and forming the aramid nano-fiber pulp obtained in the step (1) on an inclined wire paper machine to obtain aramid nano-paper, wherein the forming mass concentration is 0.04%;
(3) squeezing and drying: placing the aramid nano paper obtained in the step (2) in a squeezer to squeeze and dry, wherein the squeezing conditions are as follows: the squeezing pressure is 0.8MPa, and the squeezing time is 10 min; the drying conditions were: drying temperature: drying at 105 deg.C for 8 min.
Example 4
The preparation method of the water-dispersible aramid nanofiber provided by the embodiment comprises the following specific preparation steps:
(1) placing 1.0g of para-aramid fibrid, 1.5g of potassium hydroxide (KOH) and 500ml of dimethyl sulfoxide (DMSO) in a container, and stirring for 6 days at the temperature of 45 ℃ under a sealed condition to obtain an aramid nano-fiber dispersion liquid dispersed in a KOH/DMSO system;
(2) injecting deionized water into the aramid nano-fiber dispersion liquid dispersed in a KOH/DMSO system obtained in the step (1) under the stirring action of 2000rpm of rotation speed, and removingThe mass ratio of the sub-water to the aramid fiber is 2.5:1, the jet pressure is 8MPa, and the jet speed is 1.0ml/s, so as to obtain the dispersion in KOH/DMSO/H2Aramid nanofibers in an O mixing system;
(3) dispersing the obtained product in the step (2) in KOH/DMSO/H2Carrying out vacuum filtration on the aramid nano-fiber in the O mixed system through a 400-mesh nylon filter membrane to obtain the aramid nano-fiber;
(4) respectively and repeatedly washing the aramid nano-fiber obtained in the step (3) for 5 times by using absolute ethyl alcohol and deionized water, wherein the ratio of the volume of the absolute ethyl alcohol to the mass of the aramid fiber required in each washing is 1ml:4mg, and the mass ratio of the deionized water to the aramid fiber is 7:1, so as to obtain colloidal aramid nano-fiber;
(5) and (4) stirring the aramid nano-fiber obtained in the step (4) for 70min under the stirring action of 1300rpm, and dispersing in deionized water, wherein the dispersion concentration is controlled to be 2.0mg/ml, so as to obtain uniform and transparent water-dispersed aramid nano-fiber.
In this embodiment, a method for preparing aramid nanopaper by using the water-dispersible aramid nanofiber prepared by the above method includes the following steps:
(1) dispersing: dispersing the prepared water-dispersed aramid nano-fiber in deionized water, wherein the dispersion concentration is 2.0 mg/ml;
(2) and (3) net surfing and forming: making and forming the aramid nano-fiber pulp obtained in the step (1) on an inclined wire paper machine to obtain aramid nano-paper, wherein the forming mass concentration is 0.05%;
(3) squeezing and drying: placing the aramid nano paper obtained in the step (2) in a squeezer to squeeze and dry, wherein the squeezing conditions are as follows: the squeezing pressure is 0.9MPa, and the squeezing time is 7 min; the drying conditions were: drying temperature: drying at 100 deg.C for 10 min.
Example 5
The preparation method of the water-dispersible aramid nanofiber provided by the embodiment comprises the following specific preparation steps:
(1) placing 1.0g of para-aramid yarn fiber, 1.5g of potassium hydroxide (KOH) and 500ml of dimethyl sulfoxide (DMSO) in a container, and stirring for 7 days at 40 ℃ under a sealed condition to obtain an aramid nanofiber dispersion liquid dispersed in a KOH/DMSO system;
(2) injecting deionized water into the aramid nano-fiber dispersion liquid dispersed in a KOH/DMSO system obtained in the step (1) at high pressure under the stirring action of the rotating speed of 2200rpm, wherein the mass ratio of the deionized water to the aramid fiber is 3:1, the jet pressure is 10MPa, and the jet speed is 1.2ml/s, so as to obtain the aramid nano-fiber dispersion liquid dispersed in the KOH/DMSO/H system2Aramid nanofibers in an O mixing system;
(3) dispersing the obtained product in the step (2) in KOH/DMSO/H2Carrying out vacuum filtration on the aramid nano-fiber in the O mixed system through a 400-mesh nylon filter membrane to obtain the aramid nano-fiber;
(4) respectively and repeatedly washing the aramid nano-fiber obtained in the step (3) for 4 times by using absolute ethyl alcohol and deionized water, wherein the ratio of the volume of the absolute ethyl alcohol to the mass of the aramid fiber required by each washing is 1ml to 3.5mg, and the mass ratio of the deionized water to the aramid fiber is 6 to 1, so as to obtain a colloidal aramid nano-fiber;
(5) and (4) stirring the aramid nano-fiber obtained in the step (4) for 50min under the stirring action of 1800rpm, and dispersing in deionized water, wherein the dispersion concentration is controlled to be 2.5mg/ml, so as to obtain uniform and transparent water-dispersed aramid nano-fiber.
In this embodiment, a method for preparing aramid nanopaper by using the water-dispersible aramid nanofiber prepared by the above method includes the following steps:
(1) dispersing: dispersing the prepared water-dispersed aramid nano-fiber in deionized water, wherein the dispersion concentration is 3.0 mg/ml;
(2) and (3) net surfing and forming: manufacturing and forming the aramid nano-fiber pulp obtained in the step (1) on an inclined wire paper machine to obtain aramid nano-paper, wherein the forming mass concentration is 0.045%;
(3) squeezing and drying: placing the aramid nano paper obtained in the step (2) in a squeezer to squeeze and dry, wherein the squeezing conditions are as follows: the squeezing pressure is 0.7MPa, and the squeezing time is 9 min; the drying conditions were: drying temperature: drying at 95 deg.C for 12 min.
Example 6
The preparation method of the water-dispersible aramid nanofiber provided by the embodiment comprises the following specific preparation steps:
(1) placing 1.0g of para-aramid chopped fiber, 1.5g of potassium hydroxide (KOH) and 500ml of dimethyl sulfoxide (DMSO) in a container, and stirring for 7 days at the temperature of 30 ℃ under a sealed condition to obtain an aramid nano-fiber dispersion liquid dispersed in a KOH/DMSO system;
(2) injecting deionized water into the aramid nano-fiber dispersion liquid dispersed in a KOH/DMSO system obtained in the step (1) under the stirring action of the rotation speed of 2500rpm, wherein the mass ratio of the deionized water to the aramid fiber is 3.5:1, the jet pressure is 12MPa, and the jet speed is 1.5ml/s, so as to obtain the aramid nano-fiber dispersion liquid dispersed in the KOH/DMSO/H system2Aramid nanofibers in an O mixing system;
(3) dispersing the obtained product in the step (2) in KOH/DMSO/H2Carrying out vacuum filtration on the aramid nano-fiber in the O mixed system through a nylon filter membrane of 450 meshes to obtain the aramid nano-fiber;
(4) respectively and repeatedly washing the aramid nano-fiber obtained in the step (3) for 5 times by using absolute ethyl alcohol and deionized water, wherein the ratio of the volume of the absolute ethyl alcohol to the mass of the aramid fiber required by each washing is 1ml:2.5mg, and the mass ratio of the deionized water to the aramid fiber is 7:1, so as to obtain a colloidal aramid nano-fiber;
(5) and (4) stirring the aramid nano-fiber obtained in the step (4) for 45min under the stirring action of 2000rpm, and dispersing in deionized water, wherein the dispersion concentration is controlled to be 3.0mg/ml, so that uniform and transparent water-dispersed aramid nano-fiber is obtained.
In this embodiment, a method for preparing aramid nanopaper by using the water-dispersible aramid nanofiber prepared by the above method includes the following steps:
(1) dispersing: dispersing the prepared water-dispersed aramid nano-fiber in deionized water, wherein the dispersion concentration is 3.5 mg/ml;
(2) and (3) net surfing and forming: making and forming the aramid nano-fiber pulp obtained in the step (1) on an inclined wire paper machine to obtain aramid nano-paper, wherein the forming mass concentration is 0.055%;
(3) squeezing and drying: placing the aramid nano paper obtained in the step (2) in a squeezer to squeeze and dry, wherein the squeezing conditions are as follows: the squeezing pressure is 0.9MPa, and the squeezing time is 7 min; the drying conditions were: drying temperature: drying at 100 deg.C for 8 min.
Example 7
The preparation method of the water-dispersible aramid nanofiber provided by the embodiment comprises the following specific preparation steps:
(1) placing 1.0g of para-aramid pulp fiber, 1.5g of potassium hydroxide (KOH) and 500ml of dimethyl sulfoxide (DMSO) in a container, and stirring for 7 days at 40 ℃ under a sealed condition to obtain an aramid nanofiber dispersion liquid dispersed in a KOH/DMSO system;
(2) injecting deionized water into the aramid nano-fiber dispersion liquid dispersed in a KOH/DMSO system obtained in the step (1) under the stirring action of the rotation speed of 2800rpm, wherein the mass ratio of the deionized water to the aramid fiber is 4:1, the jet pressure is 13MPa, and the jet speed is 1.7ml/s, so as to obtain the aramid nano-fiber dispersion liquid dispersed in the KOH/DMSO/H system2Aramid nanofibers in an O mixing system;
(3) dispersing the obtained product in the step (2) in KOH/DMSO/H2Carrying out vacuum filtration on the aramid nano-fiber in the O mixed system through a 500-mesh nylon filter membrane to obtain the aramid nano-fiber;
(4) respectively and repeatedly washing the aramid nano-fiber obtained in the step (3) for 4 times by using absolute ethyl alcohol and deionized water, wherein the ratio of the volume of the absolute ethyl alcohol to the mass of the aramid fiber required in each washing is 1ml:2mg, and the mass ratio of the deionized water to the aramid fiber is 6:1, so as to obtain colloidal aramid nano-fiber;
(5) and (4) stirring the aramid nano-fiber obtained in the step (4) for 40min under the stirring action of 2300rpm, and dispersing in deionized water, wherein the dispersion concentration is controlled to be 4.0mg/ml, so as to obtain uniform and transparent water-dispersed aramid nano-fiber.
In this embodiment, a method for preparing aramid nanopaper by using the water-dispersible aramid nanofiber prepared by the above method includes the following steps:
(1) dispersing: dispersing the prepared water-dispersed aramid nano-fiber in deionized water, wherein the dispersion concentration is 4 mg/ml;
(2) and (3) net surfing and forming: making and forming the aramid nano-fiber pulp obtained in the step (1) on an inclined wire paper machine to obtain aramid nano-paper, wherein the forming mass concentration is 0.06%;
(3) squeezing and drying: placing the aramid nano paper obtained in the step (2) in a squeezer to squeeze and dry, wherein the squeezing conditions are as follows: the squeezing pressure is 0.8MPa, and the squeezing time is 8 min; the drying conditions were: drying temperature: drying at 95 deg.C for 12 min.
Example 8
The preparation method of the water-dispersible aramid nanofiber provided by the embodiment comprises the following specific preparation steps:
(1) placing 1.0g of para-aramid fibrid, 1.5g of potassium hydroxide (KOH) and 500ml of dimethyl sulfoxide (DMSO) in a container, and stirring for 7 days at the temperature of 50 ℃ under a sealed condition to obtain an aramid nano-fiber dispersion liquid dispersed in a KOH/DMSO system;
(2) injecting deionized water into the aramid nano-fiber dispersion liquid dispersed in a KOH/DMSO system obtained in the step (1) under the stirring action of 3000rpm, wherein the mass ratio of the deionized water to the aramid fiber is 5:1, the jet pressure is 15MPa, and the jet speed is 2ml/s, so as to obtain the aramid nano-fiber dispersion liquid dispersed in a KOH/DMSO/H system2Aramid nanofibers in an O mixing system;
(3) dispersing the obtained product in the step (2) in KOH/DMSO/H2Carrying out vacuum filtration on the aramid nano-fiber in the O mixed system through a 500-mesh nylon filter membrane to obtain the aramid nano-fiber;
(4) respectively and repeatedly washing the aramid nano-fiber obtained in the step (3) for 5 times by using absolute ethyl alcohol and deionized water, wherein the ratio of the volume of the absolute ethyl alcohol to the mass of the aramid fiber required in each washing is 1ml:2mg, and the mass ratio of the deionized water to the aramid fiber is 5:1, so as to obtain colloidal aramid nano-fiber;
(5) and (4) stirring the aramid nano-fiber obtained in the step (4) for 30min under the stirring action of 2500rpm, and dispersing in deionized water, wherein the dispersion concentration is controlled to be 5.0mg/ml, so as to obtain uniform and transparent water-dispersed aramid nano-fiber.
In this embodiment, a method for preparing aramid nanopaper by using the water-dispersible aramid nanofiber prepared by the above method includes the following steps:
(1) dispersing: dispersing the prepared water-dispersed aramid nano-fiber in deionized water, wherein the dispersion concentration is 5 mg/ml;
(2) and (3) net surfing and forming: making and forming the aramid nano-fiber pulp obtained in the step (1) on an inclined wire paper machine to obtain aramid nano-paper, wherein the forming mass concentration is 0.06%;
(3) squeezing and drying: placing the aramid nano paper obtained in the step (2) in a squeezer to squeeze and dry, wherein the squeezing conditions are as follows: squeezing pressure of 1.0MPa for 5 min; the drying conditions were: drying temperature: drying at 90 deg.C for 15 min.
The water dispersible aramid nano-fiber prepared in the embodiment 6 of the invention is detected and characterized, the diameter is 20.5 +/-3.4 nm, the crystallinity is 82 percent, and TG is10％532 ℃. The aramid fiber nano paper prepared by the method is detected and characterized, and part of indexes are as follows: 1. quantification: 40.0m2(ii)/g; 2. tensile strength: 97.0 MPa; 3. tear strength: 204.21 mN; 4. compressive strength: 86.3 kV/mm; 5. TG (gamma-10％: 535.6 ℃. The aramid nano-fiber prepared by the method can be completely dispersed in a water phase system or a hydrophilic solvent uniformly and stably, and has the advantages of small diameter, large length-diameter ratio, high surface activity and excellent heat resistance. The aramid nano paper prepared by using the water dispersible aramid nano fiber prepared by the method as the raw material has the advantages of good forming uniformity, compact paper structure, excellent mechanical strength and compressive strength performance and the like, and can be widely applied to the high-end electrical insulation field as a high-performance insulating material.
Claims (8)
1. The preparation method of the water dispersible aramid nanofiber is characterized by comprising the following steps:
(1) placing para-aramid fiber, potassium hydroxide and dimethyl sulfoxide into a container, and stirring and dispersing to obtain an aramid nanofiber dispersion liquid dispersed in a KOH/DMSO system;
(2) injecting deionized water into the aramid nano-fiber dispersion liquid dispersed in a KOH/DMSO system obtained in the step (1) under the stirring action at high pressure to obtain the aramid nano-fiber dispersion liquid dispersed in KOH/DMSO/H2Aramid nanofibers in an O mixing system; the jet pressure of the high-pressure injection is 5-15 MPa, and the jet speed is 0.2-2.0 mL/s; the mass ratio of the jet flow deionized water to the para-aramid fiber is 1: 1-5: 1;
(3) dispersing the obtained product in the step (2) in KOH/DMSO/H2Carrying out vacuum filtration on the aramid nano-fiber in the O mixed system to obtain the aramid nano-fiber;
(4) repeatedly washing the aramid nano-fiber obtained in the step (3) by absolute ethyl alcohol and deionized water to obtain colloidal aramid nano-fiber;
(5) and (4) dispersing the colloidal aramid nano-fiber obtained in the step (4) in deionized water under the stirring action to obtain the water-dispersed aramid nano-fiber.
2. The preparation method of the water-dispersible aramid nano-fiber according to claim 1, wherein the proportion of the para-aramid fiber, the potassium hydroxide and the dimethyl sulfoxide in the step (1) is 1 g: 1.5 g: 500ml, the para-aramid fiber is one of para-aramid yarn fiber, para-aramid chopped fiber, para-aramid pulp fiber and para-aramid fibrid.
3. The preparation method of the water-dispersible aramid nano-fiber according to claim 1, wherein the filter membrane adopted in the vacuum filtration in the step (3) is a nylon filter membrane of 200-500 meshes.
4. The preparation method of the water-dispersible aramid nano-fiber according to claim 1, wherein the ratio of the volume of the absolute ethyl alcohol for washing to the mass of the aramid fiber in the step (4) is 1mL:5 mg-1 mL:2 mg; the mass ratio of the deionized water for washing to the aramid fiber is 10: 1-5: 1.
5. The preparation method of the water-dispersible aramid nano-fiber according to claim 1, wherein the dispersion concentration of the colloidal aramid nano-fiber in deionized water in the step (5) is 0.5-5 mg/mL.
6. The preparation method of the water dispersible aramid nano-fiber according to claim 1, wherein the stirring in the step (1) is performed for 5-8 days at 30-50 ℃ under a sealed condition; in the step (2), the stirring speed is 600-3000 rpm; in the step (5), the stirring revolution is 500-2500 rpm, and the stirring time is 30-180 min.
7. A method for preparing aramid nanopaper by using the water-dispersed aramid nanofibers prepared by any one of the methods of claims 1 to 6, comprising the steps of:
(1) dispersing: dispersing water-dispersed aramid nano-fibers in deionized water to obtain aramid nano-fiber slurry, wherein the dispersion concentration is 0.2-5 mg/mL;
(2) and (3) net surfing and forming: making and forming the aramid nano-fiber pulp obtained in the step (1) on an inclined wire paper machine to obtain aramid nano-paper wet paper, wherein the forming mass concentration is 0.02-0.06%;
(3) squeezing and drying: and (3) placing the aramid fiber nano paper wet paper obtained in the step (2) in a squeezer to squeeze and dry the aramid fiber nano paper wet paper to obtain the aramid fiber nano paper.
8. The preparation method of the aramid nano paper as claimed in claim 7, wherein the pressing conditions in the step (3) are as follows: the squeezing pressure is 0.2-1.0 MPa, and the squeezing time is 3-20 min; the drying conditions are as follows: drying temperature: and drying for 5-15 min at 90-110 ℃.
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