CN106592000A - Method for producing aramid fiber III fibrid - Google Patents

Method for producing aramid fiber III fibrid Download PDF

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Publication number
CN106592000A
CN106592000A CN201611192876.6A CN201611192876A CN106592000A CN 106592000 A CN106592000 A CN 106592000A CN 201611192876 A CN201611192876 A CN 201611192876A CN 106592000 A CN106592000 A CN 106592000A
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fibrid
iii
aramid fiber
dmac
resin solution
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CN106592000B (en
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张鸥
张胜才
韩和平
冷枫
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Sichuan Huiteng Technology Co Ltd
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Sichuan Huiteng Technology Co Ltd
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/78Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
    • D01F6/80Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyamides
    • D01F6/805Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyamides from aromatic copolyamides
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G69/00Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
    • C08G69/02Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
    • C08G69/26Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
    • C08G69/32Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids from aromatic diamines and aromatic dicarboxylic acids with both amino and carboxylic groups aromatically bound
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F13/00Recovery of starting material, waste material or solvents during the manufacture of artificial filaments or the like
    • D01F13/04Recovery of starting material, waste material or solvents during the manufacture of artificial filaments or the like of synthetic polymers
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product
    • Y02P70/62Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Artificial Filaments (AREA)
  • Polyamides (AREA)

Abstract

The invention relates to the technical field of special synthetic fiber manufacturing, and concretely relates to a method for producing aramid fiber III fibrid. The method comprises the following steps: 1, carrying out low temperature copolycondensation on raw materials comprising p-phenylenediamine, paraphthaloyl chloride and an R3 monomer by adopting DMAC as a solvent and lithium chloride as a cosolvent to prepare an aramid fiber III resin synthesis solution, wherein lithium hydroxide is used as a HCl neutralizer; 2, diluting the resin solution with a solvent DMAC; 3, uniformly stirring water and the solvent DMAC to prepare a solidification liquid; 4, respectively sending the solidification liquid and the diluted resin solution to a three-level gear high-speed shearing and precipitating machine for intersecting diffusion and toothed disc shearing in order to obtain a fibrid suspension, and allowing the fibrid suspension to automatically flow into a solidification barrel; 5, carrying out solidification to obtain a semi-finished wet base fibrid; and 6, carrying out dehydration drying to obtain the finished product. The aramid fiber III fibrid is suitable for being used as a composite reinforcement, and can be used in the production of various structure members through modification granulation of the aramid fiber III fibrid and other special polymeric resins and granule injection molding, so the application range of the aramid fiber III is greatly enlarged.

Description

A kind of method for producing aramid III fibrid
Technical field
The present invention relates to specialty synthetic fibre manufacturing technology field, specially a kind of side for producing aramid III fibrid Method.
Background technology
Aramid fiber III chemistry full name heteroaromatic copolyamide, molecular structural formula is:
Aramid fiber III is (template base material, fixed with fibre bundle, tow fabric (rope, band, cloth etc.) and tow textile resins complex Type product etc.) be product display form, with lightweight, high-strength, wave transparent, anticorrosive, resistance to irradiation, high-low temperature resistant, high flame retardant and The excellent properties such as high-flexibility.Be space flight and aviation, naval vessel, auto industry, ballistic-resistant article, hawser, infrastructure and architectural engineering, The core base material of the high-end industry such as sports equipment, gas cylinder, IT industry and the strategic materials of national security, with wide Dual-use market prospect and current demand.
The production technology of aramid IIII fiber is resins synthesis → neutralization → spinning → washing → stretching → heat treatment → tow Shape product.The topmost application processing of aramid IIII fiber is that tow or fabric are used for into composite product as reinforcement Production, but the morphological character impact of fiber or fibre is limited in composite product machine-shaping production process, only Suitable for the processing mode such as hand pasting forming, Wrapping formed, composite product mostly is the routine shape such as the sheet material of standard type, cylinder Shape, it is impossible to be applied to that bulk strength has high demands, dimensional accuracy is high, the structural member production and processing of complex shape, thus limit virtue The range of application of the fiber of synthetic fibre III.Aramid IIII fiber application is processed showed low production efficiency, is limited using processing, cost performance is low The problems such as, result in commercialized development of the current aramid IIII fiber in addition to space flight military project and the civilian high-end field of minority are applied and take a step Dimension is difficult.
To solve an application processing difficult problem for aramid IIII fiber, range of application is expanded, research worker proposes aramid fiber III precipitating Fiber is researched and developed.Aramid fiber III fibrid is a differential kind of aramid IIII fiber, and chemical constitution is identical with aramid fiber III, therefore It remains aramid fiber III excellent properties most absolutely, but because the unique of its fiber forming process makes it have some districts again Not filoplume, soft cotton-shaped is not rendered as in the physical property of aramid IIII fiber, i.e. fiber, with draw ratio is appropriate, filoplumeization is rich It is rich, the features such as specific surface area is big;Using aramid fiber III fibrid as various composite material reinforcement bodies, by purposes requirement and other spies Planting macromolecule resin carries out composite modified pelletize, obtains the various enhancing pellets containing fine amount, and can pass through pellet use in injection molding In producing, bulk strength has high demands, dimensional accuracy is high, complex shape structural member, can greatly extend the application model of aramid fiber III Enclose.
The production method of aramid fiber III fibrid is different from the techniques such as existing aramid IIII fiber, aramid II fibrid, dress Standby technology.In the resin solution requirement that adopted of production aramid fiber III fibrid HCL first by resin in molten and remove, generated LiCL salt can be conducive to fiberizing control as diffusion velocity inhibitor in resin and water double diffusion fiber formation process System, while and operation acid corrosion after reducing, existed with aramid fiber III resin solution (such as CN101851809A) different from production spinning HCL, rear step H CL neutralisation treatment are removed during spinning (dry or wet);For producing the aramid fiber III resin of fibrid Because molecular weight is big, intrinsic viscosity (4.0~6.0) far above aramid II resin, poor fluidity the features such as, it is necessary to using relatively low tree Fat diluent concentration (2.0~5.0%), unconventional solidification liquid proportioning (1:20~50), multistage high shear special equipment (multi-stage gear disk, 7000-12000 rev/min of rotating speed) could form the cotton-shaped fibrid of filoplumeization, heavy different from existing aramid II Analysis fibre technology (such as CN102660795A), because intrinsic viscosity low (≤2.0), mobility can preferably adopt higher resins dilute Liquid concentration (6.0~12.0%), conventional solidification liquid proportioning (1:5.0~20.0), simply disperse former (such as single-stage tooth Disk, rotating speed is less than 6000 revs/min) can just meet technological requirement;The production of aramid fiber III fibrid adopts DMAC (N, N- dimethyl second Amide) it is solvent, lithium chloride is cosolvent, and Lithium hydrate is HCL nertralizers, and neutralized reaction product is lithium chloride, production process system It is unified, lithium chloride recycling can be reclaimed, CaCL is adopted substantially different from existing aramid fiber production system2Or LiCL and DMAC or NMP as dicyandiamide solution, and in HCL and when for cost consideration mostly adopt Ca (OH)2, rear operation solvent recovery only reclaims Solvent, to salt (CaCL2And LiCL) because of system disunity, it is impossible to recycling use is only made discharge and is disposed, and new environmental regulation Release chloride ion index request that industrial wastewater discharge is proposed will form havoc to this production system.
The content of the invention
The present invention is exactly directed to above technical problem, there is provided a kind of method for producing aramid III fibrid.Production Technique is synthetic resin → resin neutralization → resins dilute → precipitating into fibre → washing and filtering → cotton-shaped product.The method is different from The production technology of existing aramid IIII fiber, makes aramid fiber III fibrid occur with wadding fibrous form, it is adaptable to as compound increasing Qiang Ti, with other speciality polymer resin modified pelletizes, is used to produce all kinds of structural members by pellet injection mo(u)lding, greatly expands The range of application of aramid fiber III is opened up.
The technical scheme is that:
A kind of method for producing aramid III fibrid, the method is comprised the following steps:
(1) resins synthesis:With paraphthaloyl chloride, p-phenylenediamine and R3Monomer is raw material, wherein paraphthaloyl chloride, right Phenylenediamine and R3Mole be 1:0.7~0.3:0.3~0.7;With DMAC (chemical names:DMAC N,N' dimethyl acetamide) it is molten Agent, lithium chloride is cosolvent, inside contracts in polymerization reaction kettle and aggregates into aramid fiber III resin solution;Resin solution intrinsic viscosity:4.0~ 6.0.Described R3Monomer is 5 (6)-amino -2- (p-aminophenyl) benzimidazoles.
(2) resin neutralization:The resin solution of synthesis is shifted in neutralization reaction kettle, is direct plungeed into and paraphthaloyl chloride The high-purity powdery Lithium hydrate of 2.0 times of equimolar ratios.
(3) resin is dilute matches somebody with somebody:With solvent DMAC, the resin solution after dilution neutralization in dilution kettle.Resin solution quality hundred Divide specific concentration control:2.0%~5.0%;
(4) solidification liquid is prepared:Stirred configuration solidification liquid with water, solvent DMAC;Solidification liquid mass percent concentration control System:DMAC 40%~60%, water 40%~60%, gross mass percentage composition is 100%;
(5) fiberizing:Solidification liquid and letdown resin solution are respectively fed to tertiary gear and cut at a high speed in certain flow ratio Precipitation machine is cut, the diffusion that crosses in precipitation machine simultaneously forms fibrid suspension Jing after toothed disc shearing, and from flowing into bucket is solidified.It is dilute Release resin solution and solidification liquid flow proportional:1:20~50;7000~12000 revs/min of precipitation machine rotating speed;Solidification bucket precipitating is fine Dimension suspension time of repose:1~4 hour.
(6) washing and filtering:The fibrid suspension of solidification is separated and repeatedly washed with water after solidification liquid through filter washing equipment Wash fiber and obtain wet basis semi-finished product.
(7) dehydrate:Wet basis fibrid semi-finished product are further dehydrated and are dried, and obtain finished products;Baking temperature≤ 150℃;Finished products water content≤5%.
(8) in washing and filtering respectively collect reclaim containing LiCL, DMAC and H2The solution of O reclaims dress by solvent and salt Put, separate and recover LiCL, DMAC and H2O is recycled.
The aramid fiber III fibrid finished products physical and chemical index obtained by the production method is:
(1), 0.5~5mm of average fiber length, 5~20m of specific surface area2/ g, 35~65 ° of SR of beating degree, 280 DEG C of heat are received Shrinkage≤20%, finished products water content≤5%;
(2) composite (containing fine amount 25%~50%) test, with aramid fiber III fibrid as reinforcement:Tensile strength 760~970MPa, 590~677MPa of shear strength.
Compared with prior art, beneficial effects of the present invention are:
(1), aramid IIII fiber tradition occurs with tow shape or fabric shape, the enhancing as composite it is modifies plus Work is difficult, it is difficult to modified pelletize;Aramid fiber III fibrid occurs with wadding fibrous form, it is adaptable to used as composite reinforcement, with Other speciality polymer resin modified pelletizes, are used to produce all kinds of structural members by pellet injection mo(u)lding, greatly extend virtue The range of application of synthetic fibre III.
(2), aramid fiber III fibrid production is taken the direct precipitating of synthetic resin to produce product into fine washing, filtering and drying and is made For composite material reinforcement body, superbhort fiber and modification are cut into after the synthetic resin of the existing aramid IIII fiber of comparison is first spinning again For the production line of composite material reinforcement body, process simplification, production cost is decreased obviously.
Description of the drawings
Fig. 1 is the schematic flow sheet of aramid fiber III fibrid production method in the present invention.
Specific embodiment
In order that the content of the invention in the present invention easily facilitates understanding, below in conjunction with the drawings and specific embodiments to this Production method is further elaborated described in invention.But this scope for being interpreted as above-mentioned theme of the invention should not be only limitted to down State embodiment.
Embodiment 1:
A kind of method for producing aramid III fibrid, the method is comprised the following steps:
(1) resins synthesis:With paraphthaloyl chloride, p-phenylenediamine and R3Monomer (5 (6)-amino -2- (p-aminophenyl) Benzimidazole) it is raw material, wherein paraphthaloyl chloride, p-phenylenediamine, R3By 1:0.4:0.6 molar equivalent dispensing;With DMAC For solvent, lithium chloride is cosolvent, inside contracts in polymerization reaction kettle and aggregates into aramid fiber III resin solution;The resin solution that requirement is produced Intrinsic viscosity is 5.5.
(2) resin neutralization:The resin solution transfer of synthesis is directly added into and paraphthaloyl chloride 2.0 in neutralization reaction kettle The high-purity powdery Lithium hydrate of times equimolar ratio.
(3) resin is dilute matches somebody with somebody:Resin solution after DMAC dilution neutralizations is added in dilution kettle, resin quality percent concentration is made For 3.0%.
(4) solidification liquid is prepared:Water, DMAC are stirred configuration solidification liquid in dosing kettle;The quality percentage of solidification liquid Specific concentration DMAC 50%, water 50%;
(5) fiberizing:Solidification liquid presses 40 with letdown resin solution:1 flow proportional is respectively fed to tertiary gear at a high speed Shearing precipitation machine, controls in 10000 revs/min of precipitation machine precipitation machine rotating speed;Fibrid suspension is formed, is solidified from flowing into Bucket, fibrid suspension stands 2 hours.
(6) washing and filtering:Fibrid suspension is sent into filtration washing all-in-one, solidification liquid is separated and is repeatedly washed with water Fiber is washed, wet basis semi-finished product are obtained;
(7) dehydrate:Wet basis fibrid semi-finished product are further dehydrated and are dried, control baking temperature≤150 DEG C, Obtain water content≤5% finished product;
(8) in washing and filtering respectively collect reclaim containing LiCL, DMAC and H2The solution of O reclaims dress by solvent and salt Put, separate and recover LiCL, DMAC and H2O is recycled.
(9) fibrid finished products physical and chemical index is detected.
Average fiber length 2.0mm, specific surface area 10m2/ g, finished products water content≤5%;
(10), detection fibers composite product physical and chemical index.
Composite containing fine amount 40%, test are produced with aramid fiber III fibrid and polyethers thioketone:Tensile strength 900MPa, shear strength 650MPa.
Embodiment 2:
A kind of method for producing aramid III fibrid, the method is comprised the following steps:
(1) resins synthesis:With paraphthaloyl chloride, p-phenylenediamine and R3Monomer (5 (6)-amino -2- (p-aminophenyl) Benzimidazole) it is raw material, wherein paraphthaloyl chloride, p-phenylenediamine, R3By 1:0.6:0.4 molar equivalent dispensing;With DMAC For solvent, lithium chloride is cosolvent, inside contracts in polymerization reaction kettle and aggregates into aramid fiber III resin solution;The resin solution that requirement is produced Intrinsic viscosity is 4.5.
(2) resin neutralization:The resin solution transfer of synthesis is directly added into and paraphthaloyl chloride 2.0 in neutralization reaction kettle The high-purity powdery Lithium hydrate of times equimolar ratio.
(3) resin is dilute matches somebody with somebody:Resin solution after DMAC dilution neutralizations is added in dilution kettle, resin quality percent concentration is made For 3.0%.
(4) solidification liquid is prepared:Water, DMAC are stirred configuration solidification liquid in dosing kettle;The quality percentage of solidification liquid Specific concentration DMAC 50%, water 50%;
(5) fiberizing:Solidification liquid presses 30 with letdown resin solution:1 flow proportional is respectively fed to tertiary gear at a high speed Shearing precipitation machine, controls in 10000 revs/min of precipitation machine precipitation machine rotating speed;Fibrid suspension is formed, is solidified from flowing into Bucket, fibrid suspension stands 2 hours.
(6) washing and filtering:Fibrid suspension is sent into filtration washing all-in-one, solidification liquid is separated and is repeatedly washed with water Fiber is washed, wet basis semi-finished product are obtained;
(7) dehydrate:Wet basis fibrid semi-finished product are further dehydrated and are dried, control baking temperature≤150 DEG C, Obtain water content≤5% finished product;
(8) in washing and filtering respectively collect reclaim containing LiCL, DMAC and H2The solution of O reclaims dress by solvent and salt Put, separate and recover LiCL, DMAC and H2O is recycled.
(9) fibrid finished products physical and chemical index is detected.
Average fiber length 2mm, specific surface area 10m2/ g, finished products water content≤5%;
(10) detection fibers composite product physical and chemical index.
Composite containing fine amount 40%, test are produced with aramid fiber III fibrid and polyethers thioketone:Tensile strength 850MPa, shear strength 620MPa.
Embodiment 3:
A kind of method for producing aramid III fibrid, the method is comprised the following steps:
(1) resins synthesis:With paraphthaloyl chloride, p-phenylenediamine and R3Monomer (5 (6)-amino -2- (p-aminophenyl) Benzimidazole) it is raw material, wherein paraphthaloyl chloride, p-phenylenediamine, R3By 1:0.4:0.6 molar equivalent dispensing;With DMAC For solvent, lithium chloride is cosolvent, inside contracts in polymerization reaction kettle and aggregates into aramid fiber III resin solution;The resin solution that requirement is produced Intrinsic viscosity is 5.5.
(2) resin neutralization:The resin solution transfer of synthesis is directly added into and paraphthaloyl chloride 2.0 in neutralization reaction kettle The high-purity powdery Lithium hydrate of times equimolar ratio.
(3) resin is dilute matches somebody with somebody:Resin solution after DMAC dilution neutralizations is added in dilution kettle, resin quality percent concentration is made For 3.0%.
(4) solidification liquid is prepared:Water, DMAC are stirred configuration solidification liquid in dosing kettle;The quality percentage of solidification liquid Specific concentration DMAC 50%, water 50%;
(5) fiberizing:Solidification liquid presses 18 with letdown resin solution:1 flow proportional is respectively fed to tertiary gear at a high speed Shearing precipitation machine, controls in 7000 revs/min of precipitation machine precipitation machine rotating speed;Fibrid suspension is formed, from flowing into bucket is solidified, Fibrid suspension stands 2 hours.
(6) washing and filtering:Fibrid suspension is sent into filtration washing all-in-one, solidification liquid is separated and is repeatedly washed with water Fiber is washed, wet basis semi-finished product are obtained;
(7) dehydrate:Wet basis fibrid semi-finished product are further dehydrated and are dried, control baking temperature≤150 DEG C, Obtain water content≤5% finished product;
(8) in washing and filtering respectively collect reclaim containing LiCL, DMAC and H2The solution of O reclaims dress by solvent and salt Put, separate and recover LiCL, DMAC and H2O is recycled.
(9) fibrid finished products physical and chemical index is detected.
Average fiber length 8.0mm, specific surface area 3m2/ g, finished products water content≤5%;
(10), detection fibers composite product physical and chemical index.
Composite containing fine amount 40%, test are produced with aramid fiber III fibrid and polyethers thioketone:Tensile strength 650MPa, shear strength 500MPa.
Embodiment compares:
Embodiment is analyzed:
Embodiment 1 compares with embodiment 2 and shows:Under similarity condition aramid fiber III fibrid composite product stretching and Shear strength, associates with the intrinsic viscosity of aramid fiber III resin for direct ratio, i.e. intrinsic viscosity is big, the stretching of composite product and cuts Shearing stress increases;
The fibrid fibre length of the production of embodiment 3 is exceeded, and specific surface area is inadequate, with composite material base compatability Difference, the pelletize injection for being modified does not reach expected intensity requirement.Embodiment 1 compares with embodiment 3 and shows:Same intrinsic viscosity poly Resin, in fiber formation process, because aramid fiber III resin properties viscosity is far above other aramid fiber resins, Resin Flow Difference, to obtain meeting modified pelletize fibrid product, need solve precipitating fiber forming process in resins dilute, solidification liquid with it is dilute The Technologies such as liquid proportioning, shearing force control are released the problems such as match.

Claims (6)

1. a kind of method for producing aramid fiber III fibrid, it is characterised in that comprise the following steps:
(1)Resins synthesis:With p-phenylenediamine, paraphthaloyl chloride and R3Monomer is raw material, and with DMAC as solvent, lithium chloride is to help Solvent, polycondensation synthesis aramid fiber III resin solution;Resin solution intrinsic viscosity:4.0~6.0;
(2)Resin is neutralized:Direct plunge into the HCl nertralizers in high-purity powdery Lithium hydrate and in resin solution, Lithium hydrate It is 2 with the mol ratio of paraphthaloyl chloride:1;
(3)Resin is dilute to match somebody with somebody:With solvent DMAC letdown resin solution, the control of resin quality concentration:2.0%~5.0%;
(4)Solidification liquid is prepared:Stirred configuration solidification liquid with water, solvent DMAC;Solidification liquid mass concentration is controlled:DMAC 40% ~60%, water 40%~60%, gross mass percentage composition is 100%;
(5)Fiberizing:Solidification liquid and letdown resin solution are respectively fed to tertiary gear high speed shear and sink in certain flow ratio Analysis machine, the diffusion that crosses in precipitation machine simultaneously forms fibrid suspension Jing after toothed disc shearing, and from flowing into bucket is solidified;
(6)Washing and filtering:The fibrid suspension of solidification washes fiber with water and obtains after filter washing equipment, separation solidification liquid To wet basis fibrid semi-finished product;
(7)Dehydrate:Wet basis fibrid semi-finished product are further dehydrated and are dried, and obtain finished product;
(8)In washing and filtering respectively collect reclaim containing LiCL, DMAC and H2The solution of O is separated by solvent and salt retracting device Reclaim LiCL, DMAC and H2O is recycled.
2. the method for producing aramid III fibrid according to claim 1, it is characterised in that:Paraphthaloyl chloride, to benzene Diamidogen and R3Mol ratio be 1:0.7~0.3:0.3~0.7.
3. the method for producing aramid III fibrid according to claim 1, it is characterised in that:Described R3Monomer is 5 (6)- amino -2-(P-aminophenyl)Benzimidazole.
4. the method for producing aramid III fibrid according to claim 1, it is characterised in that:Step(4)Described in dilute Resin solution and solidification liquid flow proportional:1:20~50;7000~12000 revs/min of tertiary gear high speed shear precipitation machine rotating speed Clock;Solidification bucket fibrid suspension time of repose:1~4 hour.
5. the method for producing aramid III fibrid according to claim 1, it is characterised in that:Step(7)Described in it is dry Dry temperature≤150 DEG C;Finished products water content≤5%.
6. the method that aramid III fibrid is produced according to any one claim in claim 1-5, its feature exists It is in the physical and chemical index of the aramid fiber III fibrid finished products obtained by the production method:
(1), 0.5~5.0mm of average fiber length, 5~20m of specific surface area2/ g, beating degree 35~650SR, 280 DEG C of thermal contractions Rate≤20%, finished products water content≤5%;
(2), the composite with aramid fiber III fibrid as reinforcement is containing fine amount 25wt%~50wt%, and tensile strength is 760~ 970MPa, 590~677MPa of shear strength.
CN201611192876.6A 2016-12-21 2016-12-21 A method of producing aramid fiber III fibrid Active CN106592000B (en)

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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN108048938A (en) * 2018-01-17 2018-05-18 烟台泰和新材料股份有限公司 A kind of production method of p-aramid fiber fibrid
CN109321998A (en) * 2018-09-28 2019-02-12 东华大学 A kind of preparation method of poly(p-phenylene terephthalamide) PPTA fibrid
CN109440216A (en) * 2018-09-28 2019-03-08 浙江大学 A kind of functionalization aramid fiber superfine fibre and its preparation method and application
CN110144636A (en) * 2019-06-10 2019-08-20 黄河三角洲京博化工研究院有限公司 A kind of p-aramid fiber fibrid and preparation method thereof
CN115369505A (en) * 2022-07-08 2022-11-22 株洲时代新材料科技股份有限公司 Multistage dispersion disc precipitation forming device and forming process, precipitation fiber precipitation purification device and process

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