CN113737569A - Preparation method of aramid fiber spinning dope coated aramid fiber paper - Google Patents
Preparation method of aramid fiber spinning dope coated aramid fiber paper Download PDFInfo
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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
- D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
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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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- 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
- D21H15/00—Pulp or paper, comprising fibres or web-forming material characterised by features other than their chemical constitution
- D21H15/02—Pulp or paper, comprising fibres or web-forming material characterised by features other than their chemical constitution characterised by configuration
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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
- D21H19/00—Coated paper; Coating material
- D21H19/10—Coatings without pigments
- D21H19/14—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12
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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
- D21H19/00—Coated paper; Coating material
- D21H19/10—Coatings without pigments
- D21H19/14—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12
- D21H19/24—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12 comprising macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D21H19/30—Polyamides; Polyimides
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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
- D21H19/00—Coated paper; Coating material
- D21H19/80—Paper comprising more than one coating
- D21H19/84—Paper comprising more than one coating on both sides of the substrate
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Abstract
The invention discloses a preparation method of aramid fiber spinning stock solution coated aramid fiber paper, which comprises the steps of respectively defibering and dispersing meta-aramid chopped fibers and meta-aramid fibrids, mixing after defibering to obtain a slurry dispersion solution, homogenizing, filtering, dehydrating, forming, squeezing and drying the slurry dispersion solution to obtain meta-aramid base paper; dissolving m-phenylenediamine in an N, N-dimethylacetamide solvent, adding isophthaloyl dichloride under stirring, carrying out polycondensation reaction at low temperature, adding chlorine oxide generated by alkali neutralization reaction, and uniformly stirring after concentration adjustment to obtain a m-aramid spinning coating liquid; and uniformly coating the prepared meta-aramid spinning coating liquid on two sides of the meta-aramid base paper, and drying at high temperature to obtain the coated aramid paper.
Description
Technical Field
The invention relates to a polymer aramid fiber material and a papermaking coating technology, in particular to a preparation method of aramid fiber paper coated with aramid fiber spinning solution.
Background
The aramid product has excellent mechanical strength, flexibility, high temperature resistance, flame retardance, insulativity and corona resistance, and is widely applied to the aspects of high-voltage and variable-frequency motors, track traffic traction motors and the like as a high-end insulating material at present. With the development of the technology, the upgrading and upgrading of the machine provides higher performance requirements for aramid products, for example, the high-speed rail is gradually accelerated, new challenges are created for the performance of insulating paper or paperboard in high-speed rail high-voltage variable frequency motors and traffic traction motors, and insulating materials with higher breakdown strength and stronger corona resistance are needed to adapt to the operation of the machine. Generally, the porosity of the common paper is between 30% and 90%, and the pore structure of the aramid paper cannot be avoided. The presence of too many pores can have a detrimental effect on both the mechanical and insulation properties of the paper-based insulation. The more paper voids, the greater the mechanical loss. The breakdown field intensity of air is very low, and is only 3kV/mm, and the inside hole of material can further cause partial discharge moreover, and partial discharge will accelerate the ageing and the breakdown of insulator, and the bigger the inside hole of insulating material is, the more easily discharge and discharge capacity are bigger, reduce electric power system security and the stability of operation by a wide margin. In addition, the capillary action of the pores of the paper-based material may adsorb moisture in the air, further reducing the insulation performance. Therefore, the structural defects have adverse effects on the improvement of the comprehensive performance of the aramid paper and the expansion of the application field. The densification research of the aramid fiber paper-based material has important significance for improving the overall performance and safety of the aramid fiber paper.
Many researches show that the aramid paper prepared by the coating method has obvious advantages compared with aramid base paper, and the compact coating can fill the gaps on the surface of the aramid paper and enable the whole paper to be compact. The problems of serious loss and low water filtering speed caused by adding nano materials in a common method are solved, a compact coating structure can be formed on the surface of the paper, and the mechanical property and the insulating property of the coated aramid paper are improved. Chinese patent application CN111235944A proposes an aramid nanofiber coated aramid fiber and a preparation method thereof, which prepares the aramid nanofiber into a coating liquid to be uniformly coated on the surface of aramid fiber paper, so that the surface of the aramid fiber paper is more compact, and the performance of the aramid fiber paper is improved. Chinese patent application CN202010796557.6 proposes a preparation method of high-performance aramid mica insulation paper, which prepares a mixed solution by mutually wrapping high-pressure homogeneous mica powder and aramid nano-particles, and breaks through the limitation of weak bonding strength of a mica interface and an aramid interface. However, the preparation process of the aramid nano-fiber is relatively complex and relatively high in cost, and secondary pollution is generated in the preparation process, so that the industrial production is not facilitated.
Disclosure of Invention
The invention aims to provide a simple and feasible method for improving the densification degree of aramid fiber paper, so as to overcome the defects of the prior art. Meanwhile, the aramid spinning mother liquor can also avoid the problem of interface combination between fibers, and further improves the insulating property of the aramid paper.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of aramid fiber spinning dope coated aramid fiber paper comprises the following steps:
(1) preparing aramid paper: respectively defibering and dispersing meta-aramid chopped fibers and meta-aramid fibrids, mixing after defibering to obtain a slurry dispersion liquid, homogenizing, filtering, dehydrating, forming, squeezing and drying the slurry dispersion liquid to obtain meta-aramid base paper;
(2) preparing aramid fiber spinning coating liquid: dissolving m-phenylenediamine in an N, N-dimethylacetamide solvent, adding isophthaloyl dichloride under stirring, carrying out polycondensation reaction at low temperature, adding chlorine oxide generated by alkali neutralization reaction, and uniformly stirring after concentration adjustment to obtain a m-aramid spinning coating liquid;
(3) preparing aramid spinning mother liquor coating aramid paper: and uniformly coating the prepared meta-aramid spinning coating liquid on two sides of the meta-aramid base paper, and drying at high temperature to obtain the coated aramid paper.
Further, the oven-dry mass ratio of the meta-aramid fibrid and the meta-aramid chopped fiber in the step (1) is (2-4): 1.
further, before defibering, the meta-aramid chopped fibers in the step (1) are stirred and washed in a sodium dodecyl benzene sulfonate solution, and the concentration of the sodium dodecyl benzene sulfonate solution is controlled to be 1.2 multiplied by 10-3And (3) mol/L, washing at 60 ℃, washing for 30min, finally washing with clean water, shredding and drying for later use.
Further, the untwining process in the step (1) is specifically as follows: putting meta-aramid fibrid and meta-aramid chopped fiber into a defiberizer, adding 2/3 water, adding a polyoxyethylene solution with the mass concentration of 0.05% as a dispersing agent, wherein the addition amount of polyoxyethylene is 0.5% of the mass of the absolute dry meta-aramid chopped fiber, and defibering in the defiberizer for 20000r to obtain a slurry dispersion liquid.
Further, in the step (1), the drying temperature is 105 ℃, the drying time is 10min, and the quantitative amount of the obtained meta-aramid raw paper is 60g/m2。
Further, the step (2) is specifically as follows: dissolving m-phenylenediamine in N, N-dimethylacetamide solvent, cooling in ice-water bath, adding m-phthaloyl chloride into the solution three times at intervals of 10 minutes and 1/3 times, removing the ice-water bath after half an hour of the ice-water bath reaction, heating to 50 ℃, reacting for 5 hours, and then adding Ca (OH)2Neutralizing the solution to obtain the meta-aramid spinning coating liquid with the mass concentration of 10-30%.
Further, in the step (2), the initial reaction concentration of the m-phenylenediamine and the isophthaloyl chloride is 1.0mol/L, the molar ratio of the isophthaloyl chloride to the m-phenylenediamine is 1.03:1, and Ca (OH)2The concentration of the solution was 1.0 mol/L.
Further, in the step (3), the prepared meta-aramid spinning coating liquid is quickly and uniformly coated on one surface of the meta-aramid base paper by using a coater, the meta-aramid base paper is placed into a paper forming dryer for vacuum drying, and after the drying is finished, the other surface is coated by using the same method for drying.
Further, the drying conditions in step (3) are: the temperature is 105 deg.C, and the time is 10 min.
Compared with the prior art, the invention has the following beneficial technical effects:
(1) the method adopts a simple and effective coating mode to prepare the aramid paper, utilizes the meta-aramid spinning mother liquor as the coating liquid, and forms a compact coating layer on the surface of the aramid paper by some aramid polymers and the like in the meta-aramid spinning mother liquor, so that some gaps on the surface of the paper are filled, the whole paper structure is densified, the electron passing path is reduced, and the insulation and pressure resistance strength of the paper is improved.
(2) The method is based on the aramid spinning mother liquor of a simulation factory, and fully utilizes the property of the aramid spinning mother liquor to reduce the problem of untight bonding of the interfaces of the meta-aramid chopped fibers and the meta-aramid fibrids. The method is simple and easy to operate, industrialization is easy to realize, and the meta-aramid fiber for papermaking and the aramid spinning mother liquor for coating are both meta-aramid high polymer materials, so that recycling is easy to realize, and the possibility of industrial batch production is improved.
Drawings
The accompanying drawings are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
Fig. 1 is an SEM image of the surface of meta-aramid chopped fibers before and after washing with LAS, wherein (a) is the surface of the fibers before washing and (b) is the surface of the fibers after washing;
fig. 2 is an SEM image of the surface of the paper before and after coating the m-aramid paper with the m-aramid spinning mother liquor, wherein (a) is the uncoated surface of the paper and (b) is the coated surface of the paper.
Detailed Description
The invention is described in further detail below:
a preparation method of aramid fiber spinning dope coated aramid fiber paper comprises the following steps:
(1) preparing aramid paper: washing meta-aramid chopped fibers required by experiments in sodium dodecyl benzene sulfonate (LAS) solution, wherein the concentration of the LAS solution is controlled to be 1.2 multiplied by 10-3And (3) mol/L, wherein the water temperature for washing is 60 ℃, the meta-position chopped fibers are soaked, stirred and washed for about 30min, finally, the meta-position chopped fibers are washed clean by clear water and taken out, and the meta-position chopped fibers are dried for standby after being torn up. After 2/3 water is added into a defiberizing machine, a certain amount of meta-aramid fibrid and meta-aramid chopped fiber are respectively put into the defiberizing machine, wherein the absolute dry mass ratio of the meta-aramid fibrid to the meta-aramid fibrid is (2-4): 1. polyethylene oxide (PEO) solution (mass concentration of 0.05%) was added as a dispersant in an amount of 0.5% relative to absolutely dry meta-aramid chopped fibers, and the resulting fibers were fluffed in a fluffer at 20000r to obtain a slurry dispersion. And then adding the slurry dispersion liquid into a paper sheet former, homogenizing, filtering, dehydrating, forming, squeezing, and carrying out vacuum drying at 105 ℃ for 10min to obtain the meta-aramid raw paper.
(2) Preparing aramid fiber spinning coating liquid: dissolving m-phenylenediamine in DMAC (dimethylacetamide), cooling in an ice-water bath, adding isophthaloyl dichloride into the solution in three times at intervals of 10 minutes, wherein 1/3 is added each time, the initial reaction concentration of the m-phenylenediamine and the isophthaloyl dichloride is 1.0mol/L (namely the total initial reaction concentration of a system after the m-phenylenediamine and the isophthaloyl dichloride are mixed), the molar ratio of the isophthaloyl dichloride to the m-phenylenediamine is 1.03, removing the ice-water bath after the ice-water bath reaction is carried out for half an hour, heating to 50 ℃, reacting for 5 hours, and then adding Ca (OH)2Neutralization of the solution, Ca (OH)2The concentration of the solution is 1.0mol/L, and the mass concentration of the obtained coating liquid is 10-30%.
(3) Preparing aramid spinning mother liquor coating aramid paper: and (3) quickly and uniformly coating the prepared meta-aramid spinning coating liquid on one surface of meta-aramid base paper by using a coater, putting the meta-aramid spinning coating liquid into a paper forming dryer, drying the meta-aramid spinning coating liquid in vacuum at 105 ℃ for 10min, coating the other surface by using the same method after drying is finished, and drying to obtain the meta-aramid coated paper.
The present invention will be described in detail with reference to examples. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
The following detailed description is illustrative of the embodiments and is intended to provide further details of the invention. Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention.
Comparative example 1
Mixing meta-aramid fibrid and meta-aramid chopped fiber in an absolute dry mass ratio of 2:1 in a fluffer for fluffing and dispersing, pouring the slurry into a paper sheet former, homogenizing, dehydrating, forming, squeezing, and vacuum drying at 105 ℃ for 10min to obtain the meta-aramid fibrid with a quantitative of 60g/m2Meta-aramid paper.
And detecting the meta-aramid paper prepared by the implementation by using a pressure tester. The detection result shows that the compressive strength of the uncoated meta-aramid base paper is 8.7 kV/mm.
Comparative example 2
Mixing meta-aramid fibrid and meta-aramid chopped fiber in an absolute dry mass ratio of 3:1 in a fluffer for fluffing and dispersing, pouring the slurry into a paper sheet former, homogenizing, dehydrating, forming, squeezing, and vacuum drying at 105 ℃ for 10min to obtain the product with a quantitative content of 60g/m2Meta-aramid paper.
And detecting the meta-aramid paper prepared by the implementation by using a pressure tester. The detection result shows that the compressive strength of the uncoated meta-aramid base paper is 9.2 kV/mm.
Example 1
A preparation method of aramid fiber spinning dope coated aramid fiber paper comprises the following steps:
(1) preparing aramid paper: washing meta-aramid chopped fiber in sodium dodecyl benzene sulfonate (LAS) solution, wherein the concentration of LAS is controlled to be 1.2 x 10-3Soaking the meta-position chopped fibers at 60 ℃, stirring and washing for about 30min, finally washing the meta-position chopped fibers with clear water, taking out the meta-position chopped fibers, tearing the meta-position chopped fibers into pieces, and drying the pieces for later use. Adding 2/3 water into a defiberizer, respectively putting a certain amount of meta-aramid fibrid and meta-aramid chopped fiber into the defiberizer, wherein the absolute dry mass ratio of the meta-aramid fibrid to the meta-aramid fibrid is 2:1, adding a Polyoxyethylene (PEO) solution (with the mass concentration of 0.05%) serving as a dispersing agent, wherein the addition amount of the Polyoxyethylene (PEO) solution is 0.5% of the absolute dry meta-aramid chopped fiber, and defibering the meta-aramid fibrid in the defiberizer by 20000r to obtain a slurry dispersion liquid. And adding the slurry dispersion liquid into a paper sheet former, homogenizing, filtering, dehydrating, forming, squeezing, and carrying out vacuum drying at 105 ℃ for 10min to obtain the meta-aramid paper.
(2) Preparing aramid fiber spinning coating liquid: dissolving 1.08g of m-phenylenediamine in DMAC (dimethylacetamide), cooling in an ice-water bath, then adding 2.09g of isophthaloyl dichloride into the solution in three times, wherein the interval between each time is 10 minutes, 1/3 is added each time, the initial reaction concentration of the m-phenylenediamine and the isophthaloyl dichloride is 1.0mol/L, removing the ice-water bath after the ice-water bath reacts for half an hour, heating to 50 ℃, reacting for 5 hours, and then adding Ca (OH)2Neutralization of the solution, Ca (OH)2The concentration of the solution was 1.0mol/L, and the mass concentration of the obtained coating solution was 10%.
(3) Preparing aramid spinning mother liquor coating aramid paper: and (3) quickly and uniformly coating the prepared meta-aramid spinning coating liquid on one surface of meta-aramid base paper by using a coater, putting the meta-aramid spinning coating liquid into a paper forming dryer, drying the meta-aramid spinning coating liquid in vacuum at 105 ℃ for 10min, coating the other surface by using the same method after drying is finished, and drying to obtain the meta-aramid coated paper.
And detecting the aramid paper prepared by the implementation by using a pressure resistance tester. The detection result shows that the compressive strength of the aramid paper after the coating of the meta-aramid spinning mother solution is 13.7 kV/mm.
Example 2
A preparation method of aramid fiber spinning dope coated aramid fiber paper comprises the following steps:
(1) preparing aramid paper: washing meta-aramid chopped fiber in sodium dodecyl benzene sulfonate (LAS) solution, wherein the concentration of LAS is controlled to be 1.2 x 10-3The mol/L is carried out, the water temperature for washing is 60 ℃, and the meta-position chopped fibers are soaked, stirred and washedAnd (5) about 30min, finally washing with clear water, taking out, shredding, and drying for later use. Adding 2/3 water into a defiberizer, respectively putting a certain amount of meta-aramid fibrid and meta-aramid chopped fiber into the defiberizer, wherein the absolute dry mass ratio of the meta-aramid fibrid to the meta-aramid fibrid is 2:1, adding a Polyoxyethylene (PEO) solution (with the mass concentration of 0.05%) serving as a dispersing agent, wherein the addition amount of the Polyoxyethylene (PEO) solution is 0.5% of the absolute dry meta-aramid chopped fiber, and defibering the meta-aramid fibrid in the defiberizer by 20000r to obtain a slurry dispersion liquid. And adding the slurry dispersion liquid into a paper sheet former, homogenizing, filtering, dehydrating, forming, squeezing, and carrying out vacuum drying at 105 ℃ for 10min to obtain the meta-aramid paper.
(2) Preparing aramid fiber spinning coating liquid: dissolving 1.08g of m-phenylenediamine in DMAC (dimethylacetamide), cooling in an ice-water bath, then adding 2.09g of isophthaloyl dichloride into the solution in three times, wherein the interval between each time is 10 minutes, 1/3 is added each time, the initial reaction concentration of the m-phenylenediamine and the isophthaloyl dichloride is 1.0mol/L, removing the ice-water bath after the ice-water bath reacts for half an hour, heating to 50 ℃, reacting for 5 hours, and then adding Ca (OH)2Neutralization of the solution, Ca (OH)2The concentration of the solution was 1.0mol/L, and the mass concentration of the obtained coating solution was 20%.
(3) Preparing aramid spinning mother liquor coating aramid paper: and (3) quickly and uniformly coating the prepared meta-aramid spinning coating liquid on one surface of meta-aramid base paper by using a coater, putting the meta-aramid spinning coating liquid into a paper forming dryer, drying the meta-aramid spinning coating liquid in vacuum at 105 ℃ for 10min, coating the other surface by using the same method after drying is finished, and drying to obtain the meta-aramid coated paper.
And detecting the aramid paper prepared by the implementation by using a pressure resistance tester. The detection result shows that the compressive strength of the aramid paper after the coating of the meta-aramid spinning mother solution is 18.5 kV/mm.
Example 3
A preparation method of aramid fiber spinning dope coated aramid fiber paper comprises the following steps:
(1) preparing aramid paper: washing meta-aramid chopped fiber in sodium dodecyl benzene sulfonate (LAS) solution, wherein the concentration of LAS is controlled to be 1.2 x 10-3mol/L, washingThe water temperature is 60 ℃, the meta-position chopped fibers are soaked, stirred and washed for about 30min, finally, the meta-position chopped fibers are washed clean by clear water and taken out, and the meta-position chopped fibers are dried for standby after being torn up. Adding 2/3 water into a defiberizer, respectively putting a certain amount of meta-aramid fibrid and meta-aramid chopped fiber into the defiberizer, wherein the absolute dry mass ratio of the meta-aramid fibrid to the meta-aramid fibrid is 2:1, adding a Polyoxyethylene (PEO) solution (with the mass concentration of 0.05%) serving as a dispersing agent, wherein the addition amount of the Polyoxyethylene (PEO) solution is 0.5% of the absolute dry meta-aramid chopped fiber, and defibering the meta-aramid fibrid in the defiberizer by 20000r to obtain a slurry dispersion liquid. And adding the slurry dispersion liquid into a paper sheet former, homogenizing, filtering, dehydrating, forming, squeezing, and carrying out vacuum drying at 105 ℃ for 10min to obtain the meta-aramid paper.
(2) Preparing aramid fiber spinning coating liquid: dissolving 1.08g of m-phenylenediamine in DMAC (dimethylacetamide), cooling in an ice-water bath, then adding 2.09g of isophthaloyl dichloride into the solution in three times, wherein the interval between each time is 10 minutes, 1/3 is added each time, the initial reaction concentration of the m-phenylenediamine and the isophthaloyl dichloride is 1.0mol/L, removing the ice-water bath after the ice-water bath reacts for half an hour, heating to 50 ℃, reacting for 5 hours, and then adding Ca (OH)2Neutralization of the solution, Ca (OH)2The concentration of the solution was 1.0mol/L, and the mass concentration of the obtained coating solution was 30%.
(3) Preparing aramid spinning mother liquor coating aramid paper: and (3) quickly and uniformly coating the prepared meta-aramid spinning coating liquid on one surface of meta-aramid base paper by using a coater, putting the meta-aramid spinning coating liquid into a paper forming dryer, drying the meta-aramid spinning coating liquid in vacuum at 105 ℃ for 10min, coating the other surface by using the same method after drying is finished, and drying to obtain the meta-aramid coated paper.
And detecting the aramid paper prepared by the implementation by using a pressure resistance tester. The detection result shows that the compressive strength of the aramid paper after the coating of the meta-aramid spinning mother solution is 22.3 kV/mm.
Example 4
A preparation method of aramid fiber spinning dope coated aramid fiber paper comprises the following steps:
(1) preparing aramid paper: the meta-aramid chopped fiber is put into sodium dodecyl benzene sulfonate (LAS) solutionWashing with LAS concentration of 1.2 × 10-3And (3) mol/L, wherein the water temperature for washing is 60 ℃, the meta-position chopped fibers are soaked, stirred and washed for about 30min, finally, the meta-position chopped fibers are washed clean by clear water and taken out, and the meta-position chopped fibers are dried for standby after being torn up. Adding 2/3 water into a defiberizer, respectively putting a certain amount of meta-aramid fibrid and meta-aramid chopped fiber into the defiberizer, wherein the absolute dry mass ratio of the meta-aramid fibrid to the meta-aramid fibrid is 3:1, adding a Polyoxyethylene (PEO) solution (with the mass concentration of 0.05%) serving as a dispersing agent, wherein the addition amount of the Polyoxyethylene (PEO) solution is 0.5% of the absolute dry meta-aramid chopped fiber, and defibering the meta-aramid fibrid in the defiberizer by 20000r to obtain a slurry dispersion liquid. And adding the slurry dispersion liquid into a paper sheet former, homogenizing, filtering, dehydrating, forming, squeezing, and carrying out vacuum drying at 105 ℃ for 10min to obtain the meta-aramid paper.
(2) Preparing aramid fiber spinning coating liquid: dissolving 1.08g of m-phenylenediamine in DMAC (dimethylacetamide), cooling in an ice-water bath, then adding 2.09g of isophthaloyl dichloride into the solution in three times, wherein the interval between each time is 10 minutes, 1/3 is added each time, the initial reaction concentration of the m-phenylenediamine and the isophthaloyl dichloride is 1.0mol/L, removing the ice-water bath after the ice-water bath reacts for half an hour, heating to 50 ℃, reacting for 5 hours, and then adding Ca (OH)2Neutralization of the solution, Ca (OH)2The concentration of the solution was 1.0mol/L, and the mass concentration of the obtained coating solution was 30%.
(3) Preparing aramid spinning mother liquor coating aramid paper: and (3) quickly and uniformly coating the prepared meta-aramid spinning coating liquid on one surface of meta-aramid base paper by using a coater, putting the meta-aramid spinning coating liquid into a paper forming dryer, drying the meta-aramid spinning coating liquid in vacuum at 105 ℃ for 10min, coating the other surface by using the same method after drying is finished, and drying to obtain the meta-aramid coated paper.
And detecting the aramid paper prepared by the implementation by using a pressure resistance tester. The detection result shows that the compressive strength of the aramid paper after the coating of the meta-aramid spinning mother solution is 22.9 kV/mm.
Example 5
A preparation method of aramid fiber spinning dope coated aramid fiber paper comprises the following steps:
(1) preparing aramid paper:washing meta-aramid chopped fiber in sodium dodecyl benzene sulfonate (LAS) solution, wherein the concentration of LAS is controlled to be 1.2 x 10-3And (3) mol/L, wherein the water temperature for washing is 60 ℃, the meta-position chopped fibers are soaked, stirred and washed for about 30min, finally, the meta-position chopped fibers are washed clean by clear water and taken out, and the meta-position chopped fibers are dried for standby after being torn up. Adding 2/3 water into a defiberizer, respectively putting a certain amount of meta-aramid fibrid and meta-aramid chopped fiber into the defiberizer, wherein the absolute dry mass ratio of the meta-aramid fibrid to the meta-aramid fibrid is 4:1, adding a Polyoxyethylene (PEO) solution (with the mass concentration of 0.05%) serving as a dispersing agent, wherein the addition amount of the Polyoxyethylene (PEO) solution is 0.5% of the absolute dry meta-aramid chopped fiber, and defibering the meta-aramid fibrid in the defiberizer by 20000r to obtain a slurry dispersion liquid. And adding the slurry dispersion liquid into a paper sheet former, homogenizing, filtering, dehydrating, forming, squeezing, and carrying out vacuum drying at 105 ℃ for 10min to obtain the meta-aramid paper.
(2) Preparing aramid fiber spinning coating liquid: dissolving 1.08g of m-phenylenediamine in DMAC (dimethylacetamide), cooling in an ice-water bath, then adding 2.09g of isophthaloyl dichloride into the solution in three times, wherein the interval between each time is 10 minutes, 1/3 is added each time, the initial reaction concentration of the m-phenylenediamine and the isophthaloyl dichloride is 1.0mol/L, removing the ice-water bath after the ice-water bath reacts for half an hour, heating to 50 ℃, reacting for 5 hours, and then adding Ca (OH)2Neutralization of the solution, Ca (OH)2The concentration of the solution was 1.0mol/L, and the mass concentration of the obtained coating solution was 30%.
(3) Preparing aramid spinning mother liquor coating aramid paper: and (3) quickly and uniformly coating the prepared meta-aramid spinning coating liquid on one surface of meta-aramid base paper by using a coater, putting the meta-aramid spinning coating liquid into a paper forming dryer, drying the meta-aramid spinning coating liquid in vacuum at 105 ℃ for 10min, coating the other surface by using the same method after drying is finished, and drying to obtain the meta-aramid coated paper.
And detecting the aramid paper prepared by the implementation by using a pressure resistance tester. The detection result shows that the compressive strength of the aramid paper after the coating of the meta-aramid spinning mother solution is 24.5 kV/mm.
The embodiments described above are merely preferred embodiments of the present invention, and should not be considered as limitations of the present invention, and features in the embodiments and examples in the present application may be arbitrarily combined with each other without conflict. The protection scope of the present invention is defined by the claims, and includes equivalents of technical features of the claims. I.e., equivalent alterations and modifications within the scope hereof, are also intended to be within the scope of the invention.
Claims (9)
1. The preparation method of the aramid fiber spinning solution coated aramid fiber paper is characterized by comprising the following steps of:
(1) preparing aramid paper: respectively defibering and dispersing meta-aramid chopped fibers and meta-aramid fibrids, mixing after defibering to obtain a slurry dispersion liquid, homogenizing, filtering, dehydrating, forming, squeezing and drying the slurry dispersion liquid to obtain meta-aramid base paper;
(2) preparing aramid fiber spinning coating liquid: dissolving m-phenylenediamine in an N, N-dimethylacetamide solvent, adding isophthaloyl dichloride under stirring, carrying out polycondensation reaction at low temperature, adding chlorine oxide generated by alkali neutralization reaction, and uniformly stirring after concentration adjustment to obtain a m-aramid spinning coating liquid;
(3) preparing aramid spinning mother liquor coating aramid paper: and uniformly coating the prepared meta-aramid spinning coating liquid on two sides of the meta-aramid base paper, and drying at high temperature to obtain the coated aramid paper.
2. The preparation method of the aramid spinning solution coated aramid paper according to claim 1, wherein the absolute dry mass ratio of the meta-aramid fibrid to the meta-aramid chopped fiber in the step (1) is (2-4): 1.
3. the method for preparing the aramid fiber spinning solution-coated aramid fiber paper as claimed in claim 1, wherein the meta-aramid chopped fibers in the step (1) are stirred and washed in a sodium dodecylbenzenesulfonate solution before defibering, and the concentration of the sodium dodecylbenzenesulfonate solution is controlled to be 1.2 x 10-3mol/L, washing temperature is 60 ℃,washing for 30min, washing with clear water, shredding, and drying.
4. The preparation method of the aramid spinning dope-coated aramid paper according to claim 1, wherein the defibering process in the step (1) is specifically as follows: putting meta-aramid fibrid and meta-aramid chopped fiber into a defiberizer, adding 2/3 water, adding a polyoxyethylene solution with the mass concentration of 0.05% as a dispersing agent, wherein the addition amount of polyoxyethylene is 0.5% of the mass of the absolute dry meta-aramid chopped fiber, and defibering in the defiberizer for 20000r to obtain a slurry dispersion liquid.
5. The preparation method of the aramid spinning dope-coated aramid paper as claimed in claim 1, wherein the drying temperature in the step (1) is 105 ℃, the drying time is 10min, and the quantitative amount of the obtained meta-aramid base paper is 60g/m2。
6. The preparation method of the aramid spinning dope-coated aramid paper according to claim 1, wherein the step (2) is specifically as follows: dissolving m-phenylenediamine in N, N-dimethylacetamide solvent, cooling in ice-water bath, adding m-phthaloyl chloride into the solution three times at intervals of 10 minutes and 1/3 times, removing the ice-water bath after half an hour of the ice-water bath reaction, heating to 50 ℃, reacting for 5 hours, and then adding Ca (OH)2Neutralizing the solution to obtain the meta-aramid spinning coating liquid with the mass concentration of 10-30%.
7. The method for preparing aramid spinning dope-coated aramid paper as claimed in claim 6, wherein the initial reaction concentration of m-phenylene diamine and isophthaloyl chloride in step (2) is 1.0mol/L, wherein the molar ratio of isophthaloyl chloride to m-phenylene diamine is 1.03:1, Ca (OH)2The concentration of the solution was 1.0 mol/L.
8. The preparation method of the aramid spinning dope-coated aramid paper according to claim 1, wherein in the step (3), the prepared m-aramid spinning dope solution is quickly and uniformly coated on one surface of m-aramid base paper by a coater, the m-aramid base paper is placed in a paper forming dryer for vacuum drying, and after the drying is finished, the other surface is coated by the same method for drying.
9. The preparation method of the aramid spinning dope-coated aramid paper as claimed in claim 8, wherein the drying conditions in the step (3) are as follows: the temperature is 105 deg.C, and the time is 10 min.
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