CN107815741A - A kind of meta-aramid filament preparation process - Google Patents
A kind of meta-aramid filament preparation process Download PDFInfo
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- CN107815741A CN107815741A CN201711008323.5A CN201711008323A CN107815741A CN 107815741 A CN107815741 A CN 107815741A CN 201711008323 A CN201711008323 A CN 201711008323A CN 107815741 A CN107815741 A CN 107815741A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/32—Polyamides 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
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
- D01D5/14—Stretch-spinning methods with flowing liquid or gaseous stretching media, e.g. solution-blowing
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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
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Abstract
The invention discloses a kind of meta-aramid filament preparation process, it is included in the system that solvent is amide compound and carries out low-temperature polycondensation, obtain the special stoste of meta-aramid long filament, after the special stoste deaeration of long filament spinning-drawing machine will be delivered to gear pump, stoste is quantified by precision metering pump again and is squeezed into coagulating bath, the strand in coagulating bath out is wound into meta-aramid long filament finished product via processes such as drawing-off, washing, humid heat treatment, post-processings.Meta-aramid long filament made from the method for the present invention all achieves in terms of tensile strength, elongation at break, percent thermal shrinkage and crystallinity to be obviously improved.
Description
Technical field
The present invention relates to aramid fiber preparation field, and in particular to a kind of meta-aramid filament preparation process.
Background technology
Aramid fiber is a kind of tec fiber with numerous excellent properties, and it is divided into meta-aramid and p-aramid fiber.Wherein
Meta-aramid can be divided into meta-aramid chopped fiber and meta-aramid long filament again.
P-aramid fiber has the characteristic of high-strength and high-modulus, and intensity is 5~6 times of steel wire, and modulus is 2~3 times of steel wire, but again
Amount is only the 1/5 of steel wire, is widely used in the fields such as military project, Aero-Space, electromechanics, automobile, sports goods.P-aramid fiber is upper
Century, the late sixties were by U.S.'s Du Pont Developeies, merchandized handling in 1972.
Meta-aramid is that a kind of exploitation is early, occupies spy using high-temperature fibre kind wide, that yield is big, development is fast, its total amount
The second of kind fiber.Poly is the sawtooth pattern macromolecular of arranged regular, before melting just
Decompose, glass transition temperature Tg is 270 DEG C, and obvious decomposition and carbonization will not occur below 350 DEG C.When temperature is more than 400 DEG C
When, the gradual embrittlement of fiber, charing are until decompose, but will not produce molten drop；Do not prolong combustion in flame, have preferably fire-retardant
Property, limited oxygen index LOI is 29% -32%, and performance is splendid.With excellent heat-resisting quantity, good dimensional stability is excellent
Spinnability, fire line and corrosion resistance.
Meta-aramid fibers have the characteristics such as excellent heat resistance, anti-flammability, electrical insulating property, chemical stability, be aviation,
Important foundation material in the fields such as space flight, national defence, electronics, communication, environmental protection, chemical industry and ocean development.Meta-aramid is earliest
Succeeded in developing by Du Pont companies of the U.S. in nineteen fifty-seven, carry out within 1961 the market development, merchandized handling in 1967.
Meta-aramid long filament also has more preferably outward appearance, color and luster, machine in addition to the characteristic of short long and slender dimension with meta-aramid
Tool performance, it is widely used in the fields such as Aero-Space, racing car clothes, automotive hose, high-grade clothing.It is first from the du pont company whole world
Since secondary development ＆ production meta-aramid long filament, there is no very much second success development and production meta-aramid long filament of appearance in long-term
Enterprise, therefore Du Pont is in the situation of simple monopoly all the time, domestic corporation has paid height to buy meta-aramid long filament
The expense of volume.Meta-aramid long filament has the characteristics of dual-use, so Dupont is strictly controlled to the product of outlet abroad
System, this just more exacerbates the demand and supply contraction of meta-aramid long filament.
At present, the Patents of meta-aramid long filament technology of preparing are there is no, wherein, patent 1：201210594328.1 one
Kind aramid filament after-treatment device and method, relate to the after-treatment device of aramid filament.Patent 2：201410003259.1 one
Preparation method of kind original liquid coloring p-aramid fiber long filament and products thereof, is related to the preparation of original liquid coloring p-aramid fiber long filament, emphasis
Describe（1）Colouring agent is ground in polymer solvent and emulsification treatment；（2）Dry-jet wet-spinning spinning mode obtains original liquid coloring contraposition
Aramid filament.
It is of the invention to be using low temperature solution polymerization technique, wet spinning technology, meta-aramid long filament heat treatment technics
The important technology of invention, after supersolidification and drawing-off, the structure of gained is still not sufficiently stable and improved, it is necessary to enter fiber
Row high-temperature shaping increase crystallinity, enhancing intensity and rigidity.The heat treatment temperature of long filament and the control of time are lifting long filament things
The key technology of rationality energy, even in flame, the intensity and outward appearance of long filament are not also damaged, and will not more be ruptured.
The content of the invention
The purpose of the present invention is in view of the shortcomings of the prior art, there is provided a kind of meta-aramid filament preparation process, is solved
Fiber is after supersolidification and drawing-off in the prior art, and the structure of gained is still not sufficiently stable and perfect, crystallinity, intensity and rigidity
The problem of poor.
In order to achieve the above object, the technical solution adopted by the present invention there is provided a kind of meta-aramid long filament preparation side
Method, include following steps：
The first step：Prepare meta-aramid long filament polymer dope
M-phenylene diamine (MPD) and m-phthaloyl chloride equimolar ratio carry out low temperature poly condensation, and reaction temperature control range is -12~0
DEG C, viscosity is 1500~2200 Po, and the hydrogen chloride generated using ammonia neutralization reaction, neutral temperature is 5~25 DEG C, and pH value is
6.5~8.5, the described polymer dope of suitable meta-aramid long filament its molecular weight distribution requirement is as far as possible low, and preferably 160,000
Accounting between~18 ten thousand is higher than 95%.
The stoste that previous step generates is filtered with accurate filter cloth using screw pump, filter pressure is 5.5~8.6 public
Jin, the stoste after the completion of filtering are yellowish transparency liquid, chlorination salt content≤1% in polymer solution.
Second step：Spin meta-aramid long filament.
The long silk stock solution of meta-aramid prepared by above-mentioned steps is transported to Spinning Machine for Long Filament meter with gear pump via filter
Pump is measured, filtering accuracy will be controlled below 5 microns.
Utilize precision metering pump（0.05~0.28 milliliter/turn）Stoste is transported to spinning pack, spinneret hole is circle,
Aperture is 0.02~0.2 millimeter, and hole count is 100~1000.
Enter from the stoste of spinning pack extrusion in coagulating bath, extruded velocity is 3.5~30 ms/min, coagulation bath temperature
Scope is 5~10 DEG C, and concentration range is 40~50%, and coagulating bath flow velocity is 3~30 ms/min；Coagulating bath flow velocity will be slightly less than original
The extruded velocity of liquid, coagulation forming are molded using glass tube tubular type, ensure that stoste is solidified under metastable environment
Agent and the phase counterdiffusion of solvent, be advantageous to improve the mechanical performance of as-spun fibre.
Strand out is stretched into stretch bath, and draw ratio is 2~5 times, and draft temperature is 8~20 DEG C, stretching
Speed is 7~150 ms/min.
Strand out, which is entered in rinsing bowl, to be washed, and washing temperature is 35~45 DEG C, and washing time is 2~5 points
Clock, it should be noted that by the solvent washes clean in fiber.
Strand coiling out is into cylinder, then carries out humid heat treatment, and temperature is 70~180 DEG C, and humidity is 80~95%, the time
For 120~160 minutes.Humid heat treatment can improve molecules align, reduce the hole of molecule interchain.
The tow handled is post-processed again, and the purpose is to improve the mechanical performance of long filament.The temperature being heat-treated afterwards is
330~460 DEG C, speed is 10~50 ms/min, and heated time is 1.6~8.4 seconds.Because this step largely determines to grow
The final mass of silk finished product, so the requirement to equipment is higher, it is desirable to which the swing of draw roll is less than 0.02mm, the temperature control of heater
Scope is positive and negative 0.5 DEG C.
Compared with prior art, the meta-aramid long filament heat treatment technics in the present invention is the important skill of invention
Art, after supersolidification and drawing-off, the structure of gained is still not sufficiently stable and improved, it is necessary to carry out high-temperature shaping increase crystallization fiber
Degree, enhancing intensity and rigidity.The heat treatment temperature of long filament and the control of time are to lift the key technology point of yarn physical performance,
Even in flame, the intensity and outward appearance of long filament are not also damaged, and will not more be ruptured.
Brief description of the drawings
Fig. 1 is a kind of schematic flow sheet of meta-aramid filament preparation process of the present invention.
Embodiment
To further illustrate the present invention, below in conjunction with the accompanying drawings and specific embodiment is further explained to the present invention
Illustrate, but following examples only play the effect for helping to understand the present invention, can not be not understood as the further limit to the present invention
It is fixed：
Comparative example：(l) preparation of poly condensation polymer, aramid fiber 1313（That is meta-aramid long filament）By isophthalic
Dimethyl chloride (ICI) and m-phenylene diamine (MPD) (MPD) polycondensation form,
Production condensation polymer mainly has following three kinds of methods：
The first：Interface polycondensation
The m-phenylene diamine (MPD) of formula ratio is dissolved in quantitative water, adding a small amount of acid absorbent turns into aqueous phase.Again by formula ratio
ICI is dissolved in organic solvent, and then ICI solution is added in the MPD aqueous solution in strong agitation, in water and the boundary of organic phase
Reacted immediately on face, generation polymer precipitation, solid polymer is obtained after separating, washing and dry.
Second：Low-temperature solution polycondensation
M-phenylene diamine (MPD) is first dissolved in N, in N dimethyl acetamide (DMAc) solvent, under agitation plus people's m-phthaloyl chloride,
Reaction is carried out at low temperature, and is progressively warming up to reaction and is terminated.Then calcium hydroxide is added, the chlorination oxygen of neutralization reaction generation,
Solution is turned into DMAc- CaCI2 amidic-salt solution systems, adjusted through over-richness, can be directly used for wet spinning, can also led to
Peralkaline ion exchange resin removes the HCI of dereaction generation.Li Wei etc. studies shadow of the tertiary amine additive to PMIA polycondensation reactions
Ring, it is found that influence of the different structure tertiary amine to PMIA molecular weight is different, wherein being used as HCI to add a small amount of a picolines
Absorbent is the most obvious to improving PMIA molecular weight.
The third：Emulsion polycondensation method
ICI is dissolved in the organic solvent for having certain intermiscibility with water（Such as cyclohexanone）, MPD is dissolved in the water containing acid absorbent,
High-speed stirred, make to carry out in the organic phase of emulsion system that polycondensation reaction formed in stirring.The method is beneficial to heat transfer.This
Outside, also patent report has vapour-phase condensation polymerization method to prepare aromatic polyamide.
In view of Low-temperature Solution Polycondensation compared with interfacial polycondensation, emulsion polycondensation, consumes, solvent is few, and production efficiency is high, direct
The operations such as resin precipitation, washing and redissolution can be saved when carrying out spinning, mashing and film using resin solution, in production
It is more economical, so low temperature solution polymerization is widely used.Poly, solvent are prepared using low-temperature polycondensation method
For N, during N dimethyl acetamide (DMAc), there are following factors to have an impact reaction：M-phthaloyl chloride, m-phenylene diamine (MPD) purity,
Mol ratio, reaction temperature, reaction time, moisture and mixing speed in solvent etc..
(2) preparation of aramid fiber 1313, fiber can use dry spinning, wet spinning or dry-jet wet spinning to prepare.
The first：Dry spinning
The flow of dry spinning is obtained containing about 20% polymerization for the spinning solution obtained by Low-temperature Solution Polycondensation is neutralized with calcium hydroxide
The viscous fluid of thing and 9% CaCl2,150~160 DEG C of progress dry spinnings are heated to after filtering, obtain as-spun fibre because carrying
A large amount of inorganic salts, need to carry out 4~5 times of stretching after repeatedly washing at 300 DEG C or so, or it is rolled after fiber be introduced into boiling
Water-bath is stretched, dried, and 1.1 times of processing are tensioned at 300 DEG C.Dry spinning product has two kinds of long filament and chopped fiber.
Second：Wet spinning
The general flow of wet spinning is：For stoste temperature control at 22 DEG C or so, it is 1.366 that stoste, which enters bulk density, before spinning
Containing in dimethyl acetamide and CaCI2 coagulating baths, bath temperature is kept for 60 DEG C, obtained as-spun fibre after washing, in hot bath
2. 73 times are stretched, is then dried again, temperature is 130 DEG C, and 1.45 times are then redrawn on 320 DEG C of hot plate and is made
Finished product.Japanese Supreme Being people uses the method.Conex product is mainly chopped fiber, there is following kind：Regular staple, original
Liquid dyeing chopped fiber, chopped strand and high strength filaments.Wet spinning flow according to the high-strength Conex of patent introduction is：Slurries
→ coagulating bath → washing → first time wet tensile → second of wet tensile → drying → thousand stretchings → post processing.Obtained resistant fiber
Zhang Qiangdu is 5.60%~6.O% up to 8.48~9.27cN/dtex, thermal contraction of the elongation 25%~28% at 300 DEG C.
The third：Dry-jet wet spinning
Monsanto Chemicals integrate the advantages of dry-spinning and wet spinning, it is proposed that the technique of dry-jet wet-spinning.Using this technique, spinning
Draw ratio is big, and directional effect is good, and heat resistance is high.Such as wet spun fibre, percent thermal shrinkage is 80% at 400 DEG C, and dry-jet wet-spinning is fine
Dimension is less than lO%, and the zero strength temperature of wet spinning is 440 DEG C, and dry-spinning is 470 DEG C, and thousand squirt spinning and can bring up to 515 DEG C.
The technological process of production that each major company uses for：Du pont company uses low temperature solution polymerization, dry spinning, obtains
Fiber Nomex, Japanese Di Ren companies use interfacial polymerization, are redissolved, carry out spinning with inverted wet spinning device, spin fibre
Dimension is referred to as Conex；The advantages of comprehensive dry-spinning of Monsanto Company and wet spinning, proposes dry-jet wet spinning process.In addition, the Φ of the former Soviet Union
EHHnox is produced with thermoplastic extrusion method.
(3) aramid fiber 1313 copolymerization and surface are modified the fatigue durability, fire-retardant for Fanglun 1313
Property, light resistance and with the wellability of matrix resin it is still not ideal enough the problems such as, carried out substantial amounts of research both at home and abroad.
Li Wei etc. is used as Third monomer with 2,5-- chlorine paraphthaloyl chloride (DDC), by it with m-phthaloyl chloride (ICl),
M-phenylene diamine (MPD) (MPD) carries out cryogenic solution copolycondensation reaction in DMA (DMAc), has synthesized chloride substitution
The poly resin (PMIAC) of base.They introduce halogen atom in the phenyl ring upper part of aromatic polymer,
The regularity of macromolecular chain can be moderately reduced, effectively improves its anti-flammability and the wellability with matrix resin.The Ozawa of Japan
The polycondensation reaction that Shuji et al. has delivered the dihalide of the dicarboxylic acids by aromatic diamine and aromatics prepares aromatic polyamides
Patent.Lin etc. have studied the method by selecting different diamines and binary acyl chlorides to can obtain different repeat units, so that
While keeping good heat resistance, the fire resistance of material is improved.Lin etc. replaces m-phenylene diamine (MPD) using TCP, if 10%
The TCP of mass ratio replaces m-phenylene diamine (MPD), and its 5% mass loss during aging course temperature can be made to be increased to 444.5 DEG C from 260.1 DEG C.
Embodiment one：First m-phenylene diamine (MPD) is dissolved in DMAC, then adds m-phthaloyl chloride and isophthalic two by a certain percentage
Polycondensation reaction occurs for amine, and controlling reaction temperature is -5~0 DEG C, and apparent viscosity control is 1800~2000 Po, afterwards by reaction life
Into HCl mol ratio 1：1 adds ammonia, is transplanted on after deaeration in stoste storage tank.
The special stoste of long filament is transplanted on Spinning Machine for Long Filament by gear pump, entered via the spinneret that aperture is 0.05mm
In coagulating bath, coagulation bath temperature is 5~6 DEG C, and the strand come out from coagulating bath, which is entered back into 18~20 DEG C of stretch bath, to be stretched, and is drawn
Multiple is stretched for 2.2 times, and draft temperature is 17 ± 1 DEG C, then strand is washed, and washes rear humid heat treatment.
Post-processing processing is finally carried out to long filament, temperature is 390 ± 0.5 DEG C, and speed is 30 ms/min, and post processing is completed
Cylinder is coiled into winder winding, it is desirable to which bobbin shaping is good afterwards.
Embodiment two：First m-phenylene diamine (MPD) is dissolved in DMAC, then adds m-phthaloyl chloride and isophthalic two by a certain percentage
Polycondensation reaction occurs for amine, and controlling reaction temperature is -5~0 DEG C, and dynamic viscosity control is 1900~2000Po, afterwards by reaction life
Into HCl mol ratio 1：1 adds ammonia, is then separated by filtration the sal-ammoniac of generation, is transplanted on after deaeration in stoste storage tank.
The special stoste of long filament is transplanted on Spinning Machine for Long Filament by gear pump, entered via the spinneret that aperture is 0.05mm
In coagulating bath, coagulation bath temperature is 5~6 DEG C, and the strand come out from coagulating bath, which is entered back into 18~20 DEG C of stretch bath, to be stretched, and is drawn
Multiple is stretched for 2.5 times, and draft temperature is 15 ± 1 DEG C, then strand is washed, and washes rear humid heat treatment.
Post-processing processing is finally carried out to long filament, temperature is 410 ± 0.5 DEG C, and speed is 25 ms/min, and post processing is completed
Cylinder is coiled into winder winding, it is desirable to which bobbin shaping is good afterwards.
Embodiment three：The first step：Prepare meta-aramid long filament polymer dope
M-phenylene diamine (MPD) and m-phthaloyl chloride equimolar ratio carry out low temperature poly condensation, and reaction temperature control range is -12~0
DEG C, viscosity is 1500~2200 Po, and the hydrogen chloride generated using ammonia neutralization reaction, neutral temperature is 5~25 DEG C, and pH value is
6.5~8.5, accounting between described its molecular weight distribution of the polymer dope of suitable meta-aramid long filament requirement 160,000~180,000
Than being higher than 95%.
The stoste that previous step generates is filtered with accurate filter cloth using screw pump, filter pressure is 5.5~8.6 public
Jin, the stoste after the completion of filtering are yellowish transparency liquid, chlorination salt content≤1% in polymer solution.
Second step：Spin meta-aramid long filament.
The long silk stock solution of meta-aramid prepared by above-mentioned steps is transported to Spinning Machine for Long Filament meter with gear pump via filter
Pump is measured, filtering accuracy will be controlled below 5 microns.
Utilize precision metering pump（0.05~0.28 milliliter/turn）Stoste is transported to spinning pack, spinneret hole is circle,
Aperture is 0.02~0.2 millimeter, and hole count is 100~1000.
Enter from the stoste of spinning pack extrusion in coagulating bath, extruded velocity is 3.5~30 ms/min, coagulation bath temperature
Scope is 5~10 DEG C, and concentration range is 40~50%, and coagulating bath flow velocity is 3~30 ms/min；Coagulating bath flow velocity will be slightly less than original
The extruded velocity of liquid, coagulation forming are molded using glass tube tubular type, ensure that stoste is solidified under metastable environment
Agent and the phase counterdiffusion of solvent, be advantageous to improve the mechanical performance of as-spun fibre.
Strand out is stretched into stretch bath, and draw ratio is 2~5 times, and draft temperature is 8~20 DEG C, stretching
Speed is 7~150 ms/min.
Strand out, which is entered in rinsing bowl, to be washed, and washing temperature is 35~45 DEG C, and washing time is 2~5 points
Clock, it should be noted that by the solvent washes clean in fiber.
Strand coiling out is into cylinder, then carries out humid heat treatment, and temperature is 70~180 DEG C, and humidity is 80~95%, the time
For 120~160 minutes.Humid heat treatment can improve molecules align, reduce the hole of molecule interchain.
The tow handled is post-processed again, is oiled, dried, wound and finally obtain finished product, the purpose is to improve
The mechanical performance of long filament.The temperature being heat-treated afterwards be 330~460 DEG C, speed be 10~50 ms/min, heated time be 1.6~
8.4 the second.Because this step largely determines the final mass of long filament finished product, so the requirement to equipment is higher, it is desirable to drawing-off
The swing of roller is less than 0.02mm, and the temperature-control range of heater is positive and negative 0.5 DEG C.
Meta-aramid long filament heat treatment technics is the important technology of invention, fiber after supersolidification and drawing-off,
The structure of gained is still not sufficiently stable and improved, it is necessary to carry out high-temperature shaping increase crystallinity, enhancing intensity and rigidity.The heat of long filament
The control for the treatment of temperature and time are to lift the key technology point of yarn physical performance, even in flame, the intensity of long filament
Also it is not damaged with outward appearance, will not more ruptures.
Example IV：The embodiment and embodiment three are essentially identical, and its difference is the humid heat treatment, and temperature is
90~160 DEG C, humidity is 85~100%, and the time is 90~100 minutes.
Embodiment five：The embodiment and embodiment three are essentially identical, and its difference is the humid heat treatment, and temperature is
100~150 DEG C, humidity is 83~92%, and the time is 110~150 minutes.
Compared with prior art, aramid filament parameters of the invention are referring to following form：
Therefore deduce that, received using meta-aramid long filament made from the method for the present invention in tensile strength, elongation at break, heat
All achieve and be obviously improved in terms of shrinkage and crystallinity.
Embodiment described above is only that the preferred embodiment of the present invention is described, not to the model of the present invention
Enclose and be defined, on the premise of design spirit of the present invention is not departed from, skill of this area ordinary skill technical staff to the present invention
The various modifications and improvement that art scheme is made, it all should fall into the protection domain of claims of the present invention determination.
Claims (7)
- A kind of 1. meta-aramid filament preparation process, it is characterised in that：Comprise the following steps：The first step：M-phenylene diamine (MPD) and m-phthaloyl chloride are subjected to low temperature poly condensation, obtain mpd-i spinning Silk solution；Second step：The polymer dope that above-mentioned steps are obtained is extruded, coagulation forming；3rd step：Stretched, washed, humid heat treatment；4th step：Following process processing is carried out, obtains meta-aramid long filament.
- A kind of 2. meta-aramid filament preparation process according to claim 1, it is characterised in that：The polymer dope Accounting between molecular weight distribution requirement 160,000~180,000 is higher than 95%.
- A kind of 3. meta-aramid filament preparation process according to claim 1, it is characterised in that：Solidification described in second step Shaping is completed in coagulating bath, and the DMAC coagulation bath temperatures are 5~10 DEG C, and concentration is 40~50%.
- 4. coagulating bath flow velocity will be slightly less than the extruded velocity of stoste, coagulation forming is molded using glass tube tubular type.
- A kind of 5. meta-aramid filament preparation process according to claim 1, it is characterised in that：The temperature of the humid heat treatment Spend for 70~180 DEG C, humidity is 80~95%, time 120-160min.
- A kind of 6. meta-aramid filament preparation process according to claim 1, it is characterised in that：The following process includes It is heat-treated by after, the rear heat treatment temperature is 330~460 DEG C.
- A kind of 7. meta-aramid filament preparation process according to claim 1, it is characterised in that：The following process is also wrapped Include and long filament is coiled into cylinder by winder winding, the total draft multiple of the draw roll of the up- coiler is 2.1~5.5 times.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20200037686A (en) * | 2018-10-01 | 2020-04-09 | 주식회사 휴비스 | Meta-Aramid Fiber of high strength and Method for Preparing the Same |
| CN112111804A (en) * | 2020-09-17 | 2020-12-22 | 株洲时代新材料科技股份有限公司 | Meta-aromatic polyamide fiber and preparation method thereof |
| CN113652764A (en) * | 2021-07-29 | 2021-11-16 | 烟台泰和新材料股份有限公司 | Surface smooth meta-aramid filament yarn and preparation method thereof |
| CN114000219A (en) * | 2021-10-29 | 2022-02-01 | 烟台泰和新材料股份有限公司 | Water-repellent and oil-repellent meta-aramid fiber and preparation method thereof |
| CN114703554A (en) * | 2022-04-27 | 2022-07-05 | 赣州龙邦材料科技有限公司 | Efficient and practical preparation method for aramid raw pulp stretch-solidification molding |
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| CN116393110A (en) * | 2023-06-07 | 2023-07-07 | 泰和新材集团股份有限公司 | Meta-aramid fiber-based composite adsorption material and preparation method and application thereof |
| CN116393110B (en) * | 2023-06-07 | 2023-08-25 | 泰和新材集团股份有限公司 | Meta-aramid fiber-based composite adsorption material and preparation method and application thereof |
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