CN106283254A - Use the method that dry-wet spinning prepares meta-aramid long filament - Google Patents
Use the method that dry-wet spinning prepares meta-aramid long filament Download PDFInfo
- Publication number
- CN106283254A CN106283254A CN201610883366.7A CN201610883366A CN106283254A CN 106283254 A CN106283254 A CN 106283254A CN 201610883366 A CN201610883366 A CN 201610883366A CN 106283254 A CN106283254 A CN 106283254A
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- Prior art keywords
- meta
- spinning
- dry
- aramid
- long filament
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- 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
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
-
- 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
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
-
- 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
-
- 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
- D01D11/00—Other features of manufacture
-
- 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
-
- 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
-
- 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
- D01D5/16—Stretch-spinning methods using rollers, or like mechanical devices, e.g. snubbing pins
Abstract
The present invention relates to a kind of method using dry-wet spinning to prepare meta-aramid long filament, comprise: spinning solution preparation, spray webbing, solidification, hot water drawing-off, washing, immersion oil, drying, hot gas spring, thermal finalization, oil and the operation such as winding；Use the method to prepare meta-aramid long filament ratio and use wet spinning technology; spinning speed at least improves more than 2.5 times; and the meta-aramid filament surface of preparation is smooth, hole is few, good mechanical property, is a kind of new method that can be used to large-scale production meta-aramid long filament.
Description
Technical field
Belong to polymeric material field, relate to the production method of chemical fibre.Exactly relate to a kind of employing dry and wet
The method of meta-aramid long filament is prepared in method spinning.
Background technology
The spinning of chemical fibre can be divided into melt spinning and solvent spinning, and solvent spinning can be divided into again wet spinning, dry method
Spinning and wet-dry change (dry-jet wet-spinning).Dry spinning, wet spinning and dry-wet spinning are all the dense molten of employing fiber-forming polymer
Liquid forms fiber.During dry-spinning, the spinning liquid thread extruded from spinneret capillary is not to enter coagulating bath, but enters and spin
In silk path, by the effect of hot-air stream in path, making the solvent in stock solution thread quickly volatilize, the solvent evaporated steams
Vapour is taken away by hot-air stream, and stock solution solidifies while gradually sloughing solvent, and elongation becomes under the effect of winding tension
Carefully form as-spun fibre.During wet spinning, the stock solution thread extruded from spray webbing eyelet enters coagulating bath, the solvent in stock solution thread
Spreading to coagulating bath, coagulator permeates to thread, so that stock solution thread reaches critical concentration, separates out and formed in coagulating bath
Fiber, diffusion and solidification in wet spinning are physical and chemical processes.Dry-wet spinning is by the feature of dry spinning Yu wet spinning
The chemical fibre spinning method combined, during dry-wet spinning, the spinning liquid thread extruded from spinneret capillary is advanced
Entering void layer, then enter back in coagulating bath, subsequent treatment is similar with wet spinning spinning.
Meta-aramid formal name used at school is poly(isophthaloyl metaphenylene diamine), and domestic also referred to as aramid fiber 1313, meta-aramid is current height
One of kind with fastest developing speed in performance fibers, is the tec fiber of a kind of high comprehensive performance, at protective clothes, honeycomb knot
The aspects such as structure material, electrically-insulating paper and high-temperature-resistant filtering material have purposes widely, be Aero-Space, electronics, communication, environmental protection,
The important foundation material in the fields such as petrochemical industry, ocean development and high-performance apparel, meta-aramid fibre fibrid and chopped strand are
Manufacture aramid insulating paper and the basic raw material of honeycomb paper.Meta-aramid chemical constitution described in the present invention is as follows.
Meta-aramid does not has fusing point, when temperature exceedes to a certain degree, and direct carbonization, cause meta-aramid to pass through molten
Melt spinning to prepare；The production of meta-aramid fibers can use dry spinning, wet spinning and dry-wet spinning.Dry spinning
Speed is fast, efficiency is high, and fiber is without skin-core structure or the most weak skin-core structure, and gained fibre machinery performance is good, but dry spinning
Technical difficulty is big, controls to require height.Wet spinning spining technology difficulty is relatively small, and single head hole count is many, yield big, but the fiber prepared
Skin-core structure is serious, and fiber Hole is many and bore hole size big, and mechanical performance is relatively poor.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of spinning speed and is better than higher than wet spinning, fibrous mechanical property
The production method of the meta-aramid long filament of wet spinning.
In order to overcome above-mentioned technical problem, the invention provides and a kind of use dry-wet spinning to prepare meta-aramid long filament
Method, it is characterised in that comprise the steps.
(1) spinning solution prepares: be polymerized the meta-aramid resin solution that gained logarithmic viscosity number is 1.8～2.3dl/g,
Be adjusted to resin quality mark 16～21%, temperature at the meta-aramid resin solution of 60～120 DEG C, then through filtering and deaeration
Obtain spinning solution.
(2) spray webbing and solidification: in upper step, spinning solution sprays after metering from spinneret orifice vertically downward, is introduced into distance
Be the air layer of 6.5～25mm, then enter back into temperature be 15～28 DEG C, solvent quality mark be the coagulating bath of 0.1～9.5%
In be frozen into as-spun fibre, drafted 1～5 times of as-spun fibre.
(3) hot water drawing-off: gained as-spun fibre drawing-off 1～3 times in the hot water of 60～95 DEG C in upper step.
(4) washing and immersion oil: in upper step, fiber is after 50～80 DEG C of heat water-spraying's washings, entering oil preparation mass fraction is 1
～10% oil groove in impregnate and oil.
(5) dry: the fiber after oiling in upper step is dried on 110～160 DEG C of hot-rollings.
(6) hot gas spring and thermal finalization: the fiber after drying in upper step drawing-off 1～3 times on 310～400 DEG C of hot-rollings, then
Thermal finalization on follow-up mutually synthermal hot-rolling.
(7) oil and wind: the fiber in upper step winds finished product after being oiled by oiling roller.
In technique scheme, spinning solution consists of: meta-aramid resin quality mark is 16～21%, calcium chloride
Mass fraction is 4～10%, and the mass fraction of water is 2～4%, the mass fraction of N,N-dimethylacetamide (DMAc) be 65～
74%。
Precision≤5 micron in technique scheme, when spinning solution filters.
In technique scheme, the solvent in spinning solution and coagulating bath is N,N-dimethylacetamide (DMAc).
In technique scheme, coagulating bath is the aqueous solution of N,N-dimethylacetamide (DMAc).
The positive effect of the present invention is.
(1) use the present invention method prepare meta-aramid fibers than use wet spinning speed at least improve 2.5 times with
On.
(2) meta-aramid fibers smooth surface, the hole that prepared by the method for the employing present invention are few, and mechanical performance compares Wet-spinning
Silk is good.
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 present invention structural representation of used device when implementing.
Detailed description of the invention
Fig. 1 is the apparatus structure schematic diagram that the present invention uses dry-wet spinning to be used when preparing meta-aramid long filament, it
Comprise metering and spinning appts, fiberizing and the after-treatment device etc. of spinning solution；The metering of spinning solution and spinning appts
Comprise: spinning solution holding vessel 1, dosing pump 2, filter 3, filament spinning component 4, spinneret 5 etc.；Their annexation is: spin
Silk stock solution holding vessel) delivery outlet be connected by the input port of pipeline with dosing pump 2, the delivery outlet of dosing pump 2 passes through pipeline
Being connected with the input port of filter 3, the delivery outlet of filter 3 is connected by the input port of pipeline with filament spinning component 4, spray webbing
Plate 5 is positioned at the port of export of filament spinning component 4.Fiberizing comprises with after-treatment device: directive wheel 6, coagulating basin 7,1# traction machine 8,
Drawing-off bath 9,2# traction machine 10, rinsing machine 11, finishing bathtray 12, dehydrator 13, heat setting machine 14, oiling machine 15, up-coiler 16
Deng；Their position relationship is: directive wheel 6 is positioned at immediately below spinneret, and directive wheel 6 is fixed in coagulating basin 7,1# traction machine 8
It is positioned at the downstream of directive wheel 6, between 1# traction machine 8 and 2# traction machine 10, is provided with drawing-off bath 9；The downstream of 2# traction machine 10 sets
It is equipped with rinsing machine 11；The downstream of rinsing machine 11 is provided with finishing bathtray 12；The downstream of finishing bathtray 12 is provided with dehydrator 13；Dehydrator
The downstream of 13 is provided with heat setting machine 14；The downstream of heat setting machine 14 is provided with oiling machine 15, and the downstream of oiling machine 15 is provided with
Up-coiler 16.
Spinning solution holding vessel 1 to the pipeline between described filament spinning component 4 input port is provided with heat tracing, uses electricity companion
Heat.
The plate face of spinneret 5 is parallel with the coagulating bath liquid level in described coagulating basin 7, and adjustable distance scope is 3 between the two
～35mm.
Rinsing machine 11 uses fountain rinsing machine.
Finishing bathtray 12 uses immersion to oil.
Dehydrator 13 uses two roller heating, and mode of heating is electrical heating.
Two heating rollers on dehydrator 13 are respectively adopted independent drive system.
Heat setting machine 14 configures four rollers, and each roller is separately configured a driving motor, and mode of heating uses electrical heating.
Oiling machine 15 uses oiling roller to oil.
Embodiment 1.
By meta-aramid resin quality mark be 16.07%, calcium chloride mass fraction be 7.5%, the mass fraction of water be
2.43%, the mass fraction of N,N-dimethylacetamide be 74% serosity be warming up to 60 DEG C, successively through filtering accuracy be 20 microns,
The cascade filtration of 10 microns, is placed in spinning solution holding vessel 1 vacuum standing and defoaming 12 hours standby.Spinning solution holding vessel 1
In spinning solution under the conveying of dosing pump 2, first pass through the filter 3 that filtering accuracy is 5 microns after, enter filament spinning component
4, from the spinneret orifice of spinneret 5 spray, enter spacing be the air layer of 10mm, then enter back in coagulating bath be frozen into nascent
Fiber (curing condition is: temperature 28 DEG C, the DMAc aqueous solution of mass fraction 8%), drafted 5 times of as-spun fibre；As-spun fibre exists
In the hot water of drawing-off bath 9 drafted 1.2 times, hot water temperature is 90 DEG C；Rinsing machine 11 is washed away by 80 DEG C of heat water-sprayings
Salt in fiber and solvent；Fiber after washing passes through oil groove 12, and oil preparation mass fraction is 8%；Again at the dehydrator 13 of 150 DEG C
Dry on hot-rolling, then drawing-off 1.5 times, rear two roller not drawing-offs between two rollers before heat setting machine 14, keep as the second roller
Speed, the temperature of four rods controls at 375 DEG C；Fiber, after oiling machine 15 oiling roller, controls oil preparation mass fraction in fiber
It is 0.8～1%；The most rolled machine 16 winds finished product.
Sampling detection, gained meta-aramid filament breakage intensity is 4.5cn/dtex.
Embodiment 2.
By meta-aramid resin quality mark be 18.05%, calcium chloride mass fraction be 8.41%, the mass fraction of water be
2.73%, the mass fraction of N,N-dimethylacetamide be 70.80% serosity be warming up to 80 DEG C, be successively 20 micro-through filtering accuracy
Rice, the cascade filtration of 10 microns, be placed in spinning solution holding vessel 1 standing and defoaming 12 hours standby.In spinning solution holding vessel 1
Spinning solution under the conveying of dosing pump 2, first pass through the filter 3 that filtering accuracy is 5 microns after, enter filament spinning component 4,
Spraying from the spinneret orifice of spinneret 5, entering spacing is the air layer of 15mm, then enters back in coagulating bath and is frozen into nascent fibre
Dimension (curing condition is: temperature 20 DEG C, the DMAc aqueous solution of mass fraction 5%), drafted 3.5 times of as-spun fibre；As-spun fibre exists
In the hot water of drawing-off bath 9 drafted 1.5 times, hot water temperature is 80 DEG C；Rinsing machine 11 is washed away by 70 DEG C of heat water-sprayings
Salt in fiber and solvent；Fiber after washing passes through oil groove 12, and oil preparation mass fraction is 6%；Again at the dehydrator 13 of 150 DEG C
Dry on hot-rolling, then drawing-off 2 times, rear two roller not drawing-offs between two rollers before heat setting machine 14, keep as the second roller
Speed, the temperature of four rods controls at 375 DEG C；Fiber is after oiling machine 15 oiling roller, and controlling oil preparation mass fraction in fiber is
0.8～1%；The most rolled machine 16 winds finished product.
Sampling detection, gained meta-aramid filament breakage intensity is 4.8cn/dtex.
Embodiment 3.
By meta-aramid resin quality mark be 20.04%, calcium chloride mass fraction be 9.34%, the mass fraction of water be
3.03%, the mass fraction of N,N-dimethylacetamide be 67.59% serosity be warming up to 110 DEG C, successively through filtering accuracy be 20
Micron, the cascade filtration of 10 microns, be placed in spinning solution holding vessel 1 standing and defoaming 12 hours standby.Spinning solution holding vessel 1
In spinning solution under the conveying of dosing pump 2, first pass through the filter 3 that filtering accuracy is 5 microns after, enter filament spinning component
4, from the spinneret orifice of spinneret 5 spray, enter spacing be the air layer of 20mm, then enter back in coagulating bath be frozen into nascent
Fiber (curing condition is: temperature 15 DEG C, the DMAc aqueous solution of mass fraction 1%), drafted 2.8 times of as-spun fibre；As-spun fibre
In the hot water of drawing-off bath 9 drafted 2.2 times, hot water temperature is 65 DEG C；Rinsing machine 11 is washed by 60 DEG C of heat water-sprayings
Fall the salt in fiber and solvent；Fiber after washing passes through oil groove 12, and oil preparation mass fraction is 5%；Again at the dehydrator of 150 DEG C
Dry on 13 hot-rollings, then drawing-off 2.5 times, rear two roller not drawing-offs between two rollers before heat setting machine 14, keep same with the second roller
The speed of sample, the temperature of four rods controls at 375 DEG C；Fiber, after oiling machine 15 oiling roller, controls oil preparation quality in fiber and divides
Number is 0.8～1%；The most rolled machine 16 winds finished product.
Sampling detection, gained meta-aramid filament breakage intensity is 5.1cn/dtex.
The above is only the preferred technical solution of the present invention, it is noted that for those of ordinary skill in the art,
On the premise of present inventive concept, it is also possible to make some improvements and modifications, these improvements and modifications should be regarded as the present invention
Protection domain in.
Claims (5)
1. one kind uses the method that dry-wet spinning prepares meta-aramid long filament, it is characterised in that comprise the steps:
(1) spinning solution prepares: polymerization gained logarithmic viscosity number, at the meta-aramid resin solution of 1.8～2.3dl/g, adjusts
Resin mass fraction 16～21%, temperature at the meta-aramid resin solution of 60～120 DEG C, then through filtering and deaeration obtains
Spinning solution；
(2) spray webbing and solidification: in upper step, spinning solution sprays after metering from spinneret orifice vertically downward, and being introduced into distance is
The air layer of 6.5～25mm, then enter back into temperature be 15～28 DEG C, solvent quality mark be 0.1～9.5% coagulating bath in
It is frozen into as-spun fibre, drafted 1～5 times of as-spun fibre；
(3) hot water drawing-off: gained as-spun fibre drawing-off 1～3 times in the hot water of 60～95 DEG C in upper step；
(4) washing and immersion oil: in upper step, fiber is after 50～80 DEG C of heat water-spraying's washings, entering oil preparation mass fraction is 1～10%
Oil groove in impregnate and oil；
(5) dry: the fiber after oiling in upper step is dried on 110～160 DEG C of hot-rollings；
(6) hot gas spring and thermal finalization: the fiber after drying in upper step drawing-off 1～3 times on 310～400 DEG C of hot-rollings, then rear
Thermal finalization on continuous mutually synthermal hot-rolling；
(7) oil and wind: the fiber in upper step winds finished product after being oiled by oiling roller.
A kind of method using dry-wet spinning to prepare meta-aramid long filament the most according to claim 1, is characterized in that: spin
Silk stock solution consists of: meta-aramid resin quality mark is 16～21%, and calcium chloride mass fraction is 4～10%, and the quality of water is divided
Number is 2～4%, and the mass fraction of N,N-dimethylacetamide is 65～74%.
A kind of method using dry-wet spinning to prepare meta-aramid long filament the most according to claim 1, is characterized in that: spin
Precision≤5 micron when silk stock solution filters.
A kind of method using dry-wet spinning to prepare meta-aramid long filament the most according to claim 1, is characterized in that: spin
Solvent in silk stock solution and coagulating bath is DMAC N,N' dimethyl acetamide.
A kind of method using dry-wet spinning to prepare meta-aramid long filament the most according to claim 1, is characterized in that: solidifying
Gu the aqueous solution that bath is DMAC N,N' dimethyl acetamide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610883366.7A CN106283254A (en) | 2016-10-10 | 2016-10-10 | Use the method that dry-wet spinning prepares meta-aramid long filament |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610883366.7A CN106283254A (en) | 2016-10-10 | 2016-10-10 | Use the method that dry-wet spinning prepares meta-aramid long filament |
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| Publication Number | Publication Date |
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| CN106283254A true CN106283254A (en) | 2017-01-04 |
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ID=57718656
Family Applications (1)
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| CN201610883366.7A Pending CN106283254A (en) | 2016-10-10 | 2016-10-10 | Use the method that dry-wet spinning prepares meta-aramid long filament |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107815741A (en) * | 2017-07-24 | 2018-03-20 | 烟台泰和新材料股份有限公司 | A kind of meta-aramid filament preparation process |
| CN110331518A (en) * | 2019-07-31 | 2019-10-15 | 太仓市梓怡纺织有限公司 | The production technology of seaweed aryl fiber cloth |
| 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 |
| CN117107373A (en) * | 2023-10-18 | 2023-11-24 | 泰和新材集团股份有限公司 | Spinning method of differential meta-aramid filaments |
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| US3414645A (en) * | 1964-06-19 | 1968-12-03 | Monsanto Co | Process for spinning wholly aromatic polyamide fibers |
| CN101255616A (en) * | 2007-03-02 | 2008-09-03 | 上海特安纶纤维有限公司 | Method for manufacturing aromatic polysulfonamides fibre |
| CN102383218A (en) * | 2011-08-26 | 2012-03-21 | 南充易安新材料有限公司 | High strength and high modulus para-aramid fiber and preparation method thereof |
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2016
- 2016-10-10 CN CN201610883366.7A patent/CN106283254A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3414645A (en) * | 1964-06-19 | 1968-12-03 | Monsanto Co | Process for spinning wholly aromatic polyamide fibers |
| CN101255616A (en) * | 2007-03-02 | 2008-09-03 | 上海特安纶纤维有限公司 | Method for manufacturing aromatic polysulfonamides fibre |
| CN102383218A (en) * | 2011-08-26 | 2012-03-21 | 南充易安新材料有限公司 | High strength and high modulus para-aramid fiber and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107815741A (en) * | 2017-07-24 | 2018-03-20 | 烟台泰和新材料股份有限公司 | A kind of meta-aramid filament preparation process |
| CN110331518A (en) * | 2019-07-31 | 2019-10-15 | 太仓市梓怡纺织有限公司 | The production technology of seaweed aryl fiber cloth |
| 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 |
| CN117107373A (en) * | 2023-10-18 | 2023-11-24 | 泰和新材集团股份有限公司 | Spinning method of differential meta-aramid filaments |
| CN117107373B (en) * | 2023-10-18 | 2024-03-12 | 泰和新材集团股份有限公司 | Spinning method of differential meta-aramid filaments |
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