CN106245141A - The production method of high-purity meta-aramid fibre fibrid - Google Patents
The production method of high-purity meta-aramid fibre fibrid Download PDFInfo
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- CN106245141A CN106245141A CN201610694517.4A CN201610694517A CN106245141A CN 106245141 A CN106245141 A CN 106245141A CN 201610694517 A CN201610694517 A CN 201610694517A CN 106245141 A CN106245141 A CN 106245141A
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- meta
- aramid
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
- D01F6/605—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides from aromatic polyamides
-
- 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
Abstract
The present invention relates to the production method of a kind of high-purity meta-aramid fibre fibrid, belong to macromolecular material production field, including: the steps such as resin heating, the cooling of precipitating liquid, resin precipitating and washing separation；Reduce system apparent viscosity by resin heating steps, increase mobility, improve production efficiency, reduce production cost；The meta-aramid resin solution that additionally present invention uses neutralizes without calcium hydroxide, in system, the impurity such as institute's calcium ions is very little, in gained meta-aramid fibre fibrid, calcium ion content is at below 20ppm, is highly suitable as high-end meta-aramid insulating paper raw material.
Description
Technical field
Belong to polymeric material field, relate to a kind of macromolecular material production method.Exactly relate to a kind of being suitable for
Production method in the high-purity meta-aramid fibre fibrid of preparation of industrialization.
Background technology
Meta-aramid formal name used at school poly(isophthaloyl metaphenylene diamine), also referred to as aramid fiber 1313, meta-aramid is that current high-performance is fine
One of kind with fastest developing speed in dimension, is the tec fiber of a kind of high comprehensive performance, at protective clothes, honeycomb texture material
The aspects such as material, electrically-insulating paper and high-temperature-resistant filtering material have purposes widely, are Aero-Space, electronics, communication, environmental protection, oil
The important foundation material in the fields such as chemical industry, ocean development and high-performance apparel.
High-purity meta-aramid fibre fibrid is the important prerequisite preparing high-quality meta-aramid insulating paper, described in the present invention
Meta-aramid chemical constitution is as follows.
Meta-aramid fibre fibrid is to manufacture honeycomb paper and the important raw and processed materials of insulating paper, its quality and the power of honeycomb paper
Learn performance, insulating paper insulating properties closely related with mechanical property.Content of ashes (especially calcium ion content) is that meta-aramid sinks
Analyse one of important quality index, the electric property of aramid insulating paper is had a major impact, the most how to reduce meta-aramid and sink
Analysis fiber ash (especially reducing calcium ion content) is to produce to be considered important of insulating paper meta-aramid fibre fibrid
Parameter.
Chinese patent CN102660795B discloses the production method of a kind of meta-aramid fibre fibrid, and its step is as follows:
By m-diaminobenzene. and m-phthaloyl chloride at DMAc(N, N-dimethyl acetylamide) in aggregate into PMIA(poly-isophthaloyl isophthalic
Diamidogen) resin；Neutralize the hydrogen chloride gas that reaction produces；By resins dilute, in mother solution, dispersion precipitating become to meet precipitating fibre
Dimension suspension and deionized water are passed through washing filter, remove solvent, auxiliary agent and the moisture content comprised in fibrid, are met
Manufacture the fibrid of meta-position aramid fiber paper condition, the method low cost, high efficiency, process stabilizing, equipment is simple, can industrialization even
Continuous production.But this patent uses the hydrogen chloride produced in calcium hydroxide and in polymerization process, cause in system containing substantial amounts of
Calcium ion, even if being washed with deionized fibrid in subsequent step, also has calcium ion residual, and such fibrid is not
It is suitable for high-grade meta-aramid insulating paper field.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of low calcium ion residual, the life of high-purity meta-aramid fibre fibrid
Product method.
In order to solve above-mentioned technical problem, the production method of a kind of high-purity meta-aramid fibre fibrid that the present invention provides,
Comprise the following steps.
(1) resin heating: meta-aramid resin solution through heat exchanger be heated to 100 DEG C～120 DEG C standby.
(2) precipitating liquid cooling: precipitating liquid is cooled to 5 DEG C～25 DEG C through heat exchanger.
(3) resin precipitating: it is heavy that meta-aramid resin solution and precipitating liquid continuously enter the most by a certain percentage
In analysis machine, after precipitation machine high speed shear, form meta-aramid precipitating stock solution.
(4) washing separates: meta-aramid precipitating stock solution, through repeatedly washing, obtains high-purity meta-aramid precipitating after solid-liquid separation
Fiber.
Meta-aramid resin solution component in described (1st) step is: mass fraction is the poly-isophthalic diformazan of 10%～16%
Acyl m-diaminobenzene. resin, mass fraction be 79.1%～86.94% DMAC N,N' dimethyl acetamide and mass fraction be 3.06%～
The hydrogen chloride of 4.9%.
Precipitating liquid in described (2nd) step is by the DMAC N,N' dimethyl acetamide that mass fraction is 19.5%～55%, quality
Mark be 42%～80 % water and hydrogen chloride that mass fraction is 0.5%～3% composition.
Precipitating liquid in described (2nd) step can also be by the DMAC N,N' dimethyl acetamide that mass fraction is 20%～55% and
Mass fraction is the water composition of 45%～80%.
In (3rd) described step resin precipitation process, certain proportion refers to the quality of meta-aramid resin solution and precipitating liquid
Ratio is 1:20～35.
(3rd) described step resin precipitation process high speed is sheared and is referred to that shear rate is 80/S～120/S.
Use in calcium hydroxide and after meta-aramid resin solution when preparing fibrid, final calcium ion content exists
More than 2000ppm；The meta-aramid resin solution that the present invention uses neutralizes without calcium hydroxide, institute's calcium ions etc. in system
Impurity is very little, and in gained meta-aramid fibre fibrid, calcium ion content is at below 20ppm, is highly suitable as high-end meta
Aramid insulating paper raw material.
Accompanying drawing explanation
Below in conjunction with the accompanying drawings, the detailed description of the invention of the present invention is elaborated.
Fig. 1 is the process units schematic diagram that the present invention is used when implementing.
Detailed description of the invention
Embodiment 1.
The process units that the present embodiment uses is as it is shown in figure 1, this apparatus structure feature is as follows.
This process units includes serosity transmission measurement system, precipitating liquid transmission measurement system, solvent transmission measurement system, water
Wash system and precipitation machine 9 etc.；Serosity transmission measurement system includes slurry storage tank 1, slurry feeding pump 3, slurry stream gauge 5 and slurry
Liquid filter 7；Precipitating liquid transmission measurement system includes precipitating liquid holding vessel 2, precipitating liquid delivery pump 4, precipitating flow meters 6 and sinks
Analysis liquid filter 8；Solvent transmission measurement system includes solvent holding vessel 10, solvent delivery pump 11 and solvent flux meter 12.Washing
System includes rinsing machine rinsing machine 13, cleaning mixture input channel 16, compressed gas input channel 17, filtrate delivery pump 14 and filtrate
Holding vessel 15.
The annexation of process units is: the delivery outlet of slurry storage tank 1 is connected with the input port of slurry feeding pump 3,
The delivery outlet of slurry feeding pump 3 is connected with the input port of slurry stream gauge 5, and the delivery outlet of slurry stream gauge 5 filters with serosity
The input port of device 7 is connected, and the delivery outlet of serosity filter 7 is connected with the serosity input port of precipitation machine 9；Precipitating liquid holding vessel
The delivery outlet of 2 is connected with the input port of precipitating liquid delivery pump 4, the delivery outlet of precipitating liquid delivery pump 4 and precipitating flow meters 6
Input port is connected, and the delivery outlet of precipitating flow meters 6 is connected with the input port of precipitating liquid filter 8, precipitating liquid filter 8
Delivery outlet be connected with the precipitating liquid input port of precipitation machine 9；The delivery outlet of solvent holding vessel 10 is defeated with solvent delivery pump 11
Entrance is connected, and the delivery outlet of solvent delivery pump 11 is connected with the input port of solvent flux meter 12, solvent flux meter 12 defeated
Outlet is connected between the delivery outlet of precipitating liquid filter 8 and the precipitating liquid input port pipeline of precipitation machine 9；The output of precipitation machine 9
Be connected to the top of rinsing machine 13 mouthful by pipeline, rinsing machine 13 be also arranged above cleaning mixture input channel 16, rinsing machine 13
Lower section be provided with compressed gas input channel 17, the delivery outlet of rinsing machine 13 is connected with the input port of filtrate delivery pump 14, filter
The delivery outlet of liquid delivery pump 14 is connected with filtrate holding vessel 15.
Slurry feeding pump 3 selects gear pump.
Centrifugal pump selected by precipitating liquid delivery pump 4.
Centrifugal pump selected by solvent delivery pump 11.
Membrane pump selected by filtrate delivery pump 14.
(more than 95%, remaining is the mass fraction of N,N-dimethylacetamide highly concentrated solvent in solvent holding vessel 10
Water) under the effect of solvent delivery pump 11, after solvent flux meter 12 measures, enter precipitating with 100.0 mass parts flow velocitys per hour
In machine 9；(mass fraction of poly(isophthaloyl metaphenylene diamine) resin is meta-aramid resin solution in slurry storage tank 1
16%, the mass fraction of N,N-dimethylacetamide is 79.1%, and the mass fraction of hydrogen chloride is 4.9%) it is heated to 120 DEG C, at slurry
Enter slurry stream gauge 5 under the effect of liquid delivery pump 3, enter filtering accuracy for 10 with 41.75 mass parts per hour after metering
The serosity filter of micron, enters back into after filtration in precipitation machine, after resin solution enters precipitation machine 9, closes solvent metering defeated
Send system, open precipitating liquid transmission measurement system；Precipitating liquid transmission measurement system feature is as follows: the precipitating of precipitating liquid holding vessel 2
Liquid (mass fraction of N,N-dimethylacetamide is 55%, and the mass fraction of water is 42%, and the mass fraction of hydrogen chloride is 3%) is cold
But to 5 DEG C, under the effect of precipitating liquid delivery pump 4, precipitating flow meters 6 is entered, then through precipitating that filtering accuracy is 1 micron
Liquid filter 8, enters in precipitation machine 9 with 1461.25 mass parts per hour (resin solution and precipitating liquid mass ratio are as 1:35), heavy
Analysis machine shear rate is 120/S, after gained fibrid stock solution scrubbed liquid (deionized water) cyclic washing 10 times, and solid-liquid separation
Obtain meta-aramid fibre fibrid.
Sampled chemical examination detection, gained meta-aramid fibre fibrid ash is 0.05%, iron ion content 10.66ppm, calcium
Ion concentration 17.43ppm.
Embodiment 2.
The present embodiment uses enforcement device same as in Example 1, and technological parameter is different.
(more than 95%, remaining is the mass fraction of N,N-dimethylacetamide highly concentrated solvent in solvent holding vessel 10
Water) under the effect of solvent delivery pump 11, after solvent flux meter 12 measures, enter precipitating with 80.0 mass parts flow velocitys per hour
In machine 9；(mass fraction of poly(isophthaloyl metaphenylene diamine) resin is meta-aramid resin solution in slurry storage tank 1
14%, the mass fraction of N,N-dimethylacetamide is 81.7%, and the mass fraction of hydrogen chloride is 4.29%) it is heated to 110 DEG C,
Entering slurry stream gauge 5 under the effect of slurry feeding pump 3, entering filtering accuracy with 47.69 mass parts per hour after metering is
The serosity filter of 10 microns, enters back in precipitation machine 9 after filtration, after resin solution enters precipitation machine 9, close solvent metering
Induction system, opens precipitating liquid transmission measurement system；Precipitating liquid transmission measurement system feature is as follows: sinking of precipitating liquid holding vessel 2
(mass fraction of N,N-dimethylacetamide is 19.5% to analysis liquid, and the mass fraction of water is 80%, and the mass fraction of hydrogen chloride is
0.5%) being cooled to 10 DEG C, enter precipitating flow meters 6 under the effect of precipitating liquid delivery pump 4, it is 1 micro-for entering back into filtering accuracy
The precipitating liquid filter 8 of rice, enters precipitating with 1430.7 mass parts per hour (resin solution and precipitating liquid mass ratio are as 1:30)
In machine 9, precipitation machine shear rate is 100/S, after gained fibrid stock solution scrubbed liquid (deionized water) cyclic washing 10 times,
Solid-liquid separation obtains meta-aramid fibre fibrid.
Sampled chemical examination detection, gained meta-aramid fibre fibrid ash is 0.05%, iron ion content 11.34ppm, calcium
Ion concentration 15.76ppm.
Embodiment 3.
The present embodiment uses enforcement device same as in Example 1, and technological parameter is different.
(more than 95%, remaining is the mass fraction of N,N-dimethylacetamide highly concentrated solvent in solvent holding vessel 10
Water) under the effect of solvent delivery pump 11, after solvent flux meter 12 measures, enter precipitating with 60.0 mass parts flow velocitys per hour
In machine 9；(mass fraction of poly(isophthaloyl metaphenylene diamine) resin is meta-aramid resin solution in slurry storage tank 1
10%, the mass fraction of N,N-dimethylacetamide is 86.94%, and the mass fraction of hydrogen chloride is 3.06%) it is heated to 100 DEG C,
Entering slurry stream gauge 5 under the effect of slurry feeding pump 3, entering filtering accuracy with 66.81 mass parts per hour after metering is
The serosity filter of 10 microns, enters back in precipitation machine 9 after filtration, after resin solution enters precipitation machine 9, close solvent metering
Induction system, opens precipitating liquid transmission measurement system；Precipitating liquid transmission measurement system feature is as follows: sinking of precipitating liquid holding vessel 2
Analysis liquid (mass fraction of N,N-dimethylacetamide is 25%, and the mass fraction of water is 75%) is cooled to 20 DEG C, defeated at precipitating liquid
Send entrance precipitating flow meters 6 under the effect of pump 4, enter back into the precipitating liquid filter 8 that filtering accuracy is 1 micron, with per hour
1336.2 mass parts (resin solution and precipitating liquid mass ratio are 1:20) enter in precipitation machine 9, and precipitation machine shear rate is 100/
S, after gained fibrid stock solution scrubbed liquid (deionized water) cyclic washing 10 times, it is fine that solid-liquid separation obtains meta-aramid precipitating
Dimension.
Sampled chemical examination detection, gained meta-aramid fibre fibrid ash is 0.05%, iron ion content 14.12ppm, calcium
Ion concentration 18.32ppm.
Embodiment 4.
The present embodiment uses enforcement device same as in Example 1, and technological parameter is different.
(more than 95%, remaining is the mass fraction of N,N-dimethylacetamide highly concentrated solvent in solvent holding vessel 10
Water) under the effect of solvent delivery pump 11, after solvent flux meter 12 measures, enter precipitating with 80.0 mass parts flow velocitys per hour
In machine 9；(mass fraction of poly(isophthaloyl metaphenylene diamine) resin is meta-aramid resin solution in slurry storage tank 1
14%, the mass fraction of N,N-dimethylacetamide is 81.7%, and the mass fraction of hydrogen chloride is 4.29%) it is heated to 110 DEG C,
Entering slurry stream gauge 5 under the effect of slurry feeding pump 3, entering filtering accuracy with 47.69 mass parts per hour after metering is
The serosity filter of 10 microns, enters back in precipitation machine 9 after filtration, after resin solution enters precipitation machine 9, close solvent metering
Induction system, opens precipitating liquid transmission measurement system；Precipitating liquid transmission measurement system feature is as follows: sinking of precipitating liquid holding vessel 2
Analysis liquid (mass fraction of N,N-dimethylacetamide is 55%, and the mass fraction of water is 45%) is cooled to 10 DEG C, defeated at precipitating liquid
Send entrance precipitating flow meters 6 under the effect of pump 4, enter back into the precipitating liquid filter 8 that filtering accuracy is 1 micron, with per hour
1430.7 mass parts (resin solution and precipitating liquid mass ratio are 1:30) enter in precipitation machine 9, and precipitation machine shear rate is 100/
S, after gained fibrid stock solution scrubbed liquid (deionized water) cyclic washing 10 times, it is fine that solid-liquid separation obtains meta-aramid precipitating
Dimension.
Sampled chemical examination detection, gained meta-aramid fibre fibrid ash is 0.05%, iron ion content 13.55ppm, calcium
Ion concentration 12.29ppm.
Comparative example 1.
The present embodiment uses enforcement device same as in Example 1, and meta-aramid resin solution neutralizes through calcium hydroxide
Process.
(more than 95%, remaining is the mass fraction of N,N-dimethylacetamide highly concentrated solvent in solvent holding vessel 10
Water) under the effect of solvent delivery pump 11, after solvent flux meter 12 measures, enter precipitating with 80.0 mass parts flow velocitys per hour
In machine 9；(mass fraction of poly(isophthaloyl metaphenylene diamine) resin is meta-aramid resin solution in slurry storage tank 1
14%, the mass fraction of N,N-dimethylacetamide is 77.35%, and the mass fraction of calcium chloride is 6.53%, and the mass fraction of water is
2.12%) it is heated to 110 DEG C, under the effect of slurry feeding pump 3, enters slurry stream gauge 5, after metering with per hour 47.69
Mass parts enters the serosity filter that filtering accuracy is 10 microns, enters back in precipitation machine 9 after filtration, and it is heavy to enter at resin solution
After analysis machine 9, close solvent transmission measurement system, open precipitating liquid transmission measurement system；Precipitating liquid transmission measurement system feature is such as
Under: the precipitating liquid (mass fraction of N,N-dimethylacetamide is 55%, and the mass fraction of water is 45%) of precipitating liquid holding vessel 2 is cold
But to 10 DEG C, under the effect of precipitating liquid delivery pump 4, enter precipitating flow meters 6, enter back into the precipitating that filtering accuracy is 1 micron
Liquid filter 8, enters in precipitation machine 9 with 1430.7 mass parts per hour (resin solution and precipitating liquid mass ratio are as 1:30), heavy
Analysis machine shear rate is 100/S, after gained fibrid stock solution scrubbed liquid (deionized water) cyclic washing 10 times, and solid-liquid separation
Obtain meta-aramid fibre fibrid.
Sampled chemical examination detection, gained meta-aramid fibre fibrid ash is 0.23%, iron ion content 260.8ppm, calcium
Ion concentration 3540ppm.
Claims (5)
1. the production method of a high-purity meta-aramid fibre fibrid, it is characterised in that: comprise the following steps:
(1) resin heating: meta-aramid resin solution through heat exchanger be heated to 100 DEG C～120 DEG C standby；
(2) precipitating liquid cooling: precipitating liquid is cooled to 5 DEG C～25 DEG C through heat exchanger；
(3) resin precipitating: meta-aramid resin solution and precipitating liquid continuously enter precipitation machine the most by a certain percentage
In, after precipitation machine high speed shear, form meta-aramid precipitating stock solution；
(4) washing separates: meta-aramid precipitating stock solution, through repeatedly washing, obtains high-purity meta-aramid precipitating fine after solid-liquid separation
Dimension；
Meta-aramid resin solution component described in above-mentioned (1st) step is: mass fraction is the poly-isophthalic diformazan of 10%～16%
Acyl m-diaminobenzene. resin, mass fraction be 79.1%～86.94% DMAC N,N' dimethyl acetamide and mass fraction be 3.06%～
The hydrogen chloride of 4.9%.
The production method of a kind of high-purity meta-aramid fibre fibrid the most according to claim 1, it is characterised in that: described
(2) the precipitating liquid in step is to be 42%～80 % by the DMAC N,N' dimethyl acetamide that mass fraction is 19.5%～55%, mass fraction
Water and hydrogen chloride that mass fraction is 0.5%～3% composition.
The production method of a kind of high-purity meta-aramid fibre fibrid the most according to claim 1, it is characterised in that: described
(2) the precipitating liquid in step is to be 45%～80% by the DMAC N,N' dimethyl acetamide that mass fraction is 20%～55% and mass fraction
Water forms.
The production method of a kind of high-purity meta-aramid fibre fibrid the most according to claim 1, it is characterised in that: described
In (3rd) step resin precipitation process, certain proportion refers to that meta-aramid resin solution is 1:20～35 with the mass ratio of precipitating liquid.
The production method of a kind of high-purity meta-aramid fibre fibrid the most according to claim 1, it is characterised in that: described
(3rd) step resin precipitation process high speed is sheared and is referred to that shear rate is 80/S～120/S.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115787123A (en) * | 2022-09-16 | 2023-03-14 | 株洲时代华先材料科技有限公司 | Meta-aramid fibrid with centralized length distribution and high water retention value and preparation method thereof |
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| CN102174771A (en) * | 2011-01-28 | 2011-09-07 | 钟洲 | Method for making additive meta-aramid paper |
| CN102660795A (en) * | 2012-05-29 | 2012-09-12 | 四川力通复合材料科技有限公司 | Production method of meta-position aramid paper fibrid |
| CN104790056A (en) * | 2015-04-15 | 2015-07-22 | 南通大学 | Preparation method for aramid fibrid |
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2016
- 2016-08-22 CN CN201610694517.4A patent/CN106245141A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1475514A (en) * | 2002-08-12 | 2004-02-18 | 东华大学 | preparation method of para Fanglun slurry cake |
| CN102174771A (en) * | 2011-01-28 | 2011-09-07 | 钟洲 | Method for making additive meta-aramid paper |
| CN102660795A (en) * | 2012-05-29 | 2012-09-12 | 四川力通复合材料科技有限公司 | Production method of meta-position aramid paper fibrid |
| CN104790056A (en) * | 2015-04-15 | 2015-07-22 | 南通大学 | Preparation method for aramid fibrid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115787123A (en) * | 2022-09-16 | 2023-03-14 | 株洲时代华先材料科技有限公司 | Meta-aramid fibrid with centralized length distribution and high water retention value and preparation method thereof |
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Application publication date: 20161221 |