CN104451935A - Solidification method for preparing para-aramid by adopting dry jet-wet spinning - Google Patents
Solidification method for preparing para-aramid by adopting dry jet-wet spinning Download PDFInfo
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- CN104451935A CN104451935A CN201410767650.9A CN201410767650A CN104451935A CN 104451935 A CN104451935 A CN 104451935A CN 201410767650 A CN201410767650 A CN 201410767650A CN 104451935 A CN104451935 A CN 104451935A
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- aramid fiber
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Abstract
The invention provides a solidification method for preparing para-aramid by adopting dry jet-wet spinning. The method is characterized by comprising the following specific steps: extruding a PPTA-H2SO4 spinning solution from a spinneret plate; enabling liquid flow extruded from the spinneret plate to vertically pass through an air layer and feeding to a solidification bath; leading out through a godet wheel, so as to obtain a nascent fiber; and washing, winding and drying, so as to obtain a para-aramid fiber precursor, wherein the solidification bath is sulfuric acid solution and is formed by sulfuric acid and water; the mass fraction of the solidification bath is 2.0%-15.0%; and the temperature of the solidification bath is 1-12 DEG C. The fineness of the fiber can be significantly reduced under the condition of the solidification bath; the strength of the para-aramid fiber is improved; the apparent defects of the fiber can be reduced; and the fiber quality is improved, thus the stability of a spinning process and the quality of a fiber product can be effectively improved.
Description
Technical field
The present invention relates to a kind of spinning technique of para-aramid fiber, more particularly, what the present invention relates to is adopt dry spray-wet method to manufacture p-aramid fiber about the research of coagulating bath, belongs to chemical synthetic fiber technical field.
Background technology
Aramid fiber has the premium properties such as high strength, high-modulus, high temperature resistant, resistance to chemical attack, quality be light, wherein specific strength is firm 5 ~ 6 times, specific modulus is 2 ~ 3 times of steel wire and glass fibre, and toughness is 2 times of steel wire, and quality is only about 1/5 of steel wire.Being one of three large high-performance fibers, being widely used in the field such as outsourcing of Aero-Space, information industry, bulletproof jacket, optical cable, is indispensable new material in national economic development and national defense construction.
P-aramid fiber is a Typical Representative in aramid fiber, first successfully developed in 1972 annual rates by du pont company, its commodity are called Kevlar, domestic related scientific research unit and institutes, the research of para-aramid fiber is carried out the sixties in 20th century, grasped key technology and equipment and the technique of p-aramid fiber production at present, relevant enterprise utilizes this technology to achieve the industrialization of para-aramid fiber.
Chinese invention 201310494251 discloses solidification forming method and the device that a kind of dry spray-wet method manufactures aramid III fiber, the method comprises as-spun fibre and solidifies stretch orientation and rapid solidification in pipe U-shaped, its spinning speed is very fast, and the fibre solidification time is shorter.But at present not about the concrete introduction of dry spray-wet-layer preparation para-aramid fiber clotting method, and coagulating bath concentration, setting temperature, setting time and air section height etc. greatly have impact on intensity and the surface topography of as-spun fibre, therefore urgently provide a kind of solidification forming method being applicable to p-aramid fiber.
Summary of the invention
The object of the invention is to improve the coagulating bath manufacturing p-aramid fiber for dry spray-wet spinning, the parameters of extraordinary coagulating bath is set, obtain higher-strength, surface is more smooth and internal structure is fine and close as-spun fibre, and can spinning continuously and stably, provide guarantee for preparing high-quality p-aramid fiber precursor further.
In order to achieve the above object, the invention provides a kind of solidification forming method that dry-wet spinning prepares p-aramid fiber, it is characterized in that, concrete steps comprise: by PPTA-H
2sO
4spinning solution is extruded from spinnerets, by the liquid stream extruded from spinnerets vertically through air layer, enter in coagulating bath, drawn by godet roller, obtain as-spun fibre, through washing, obtain para-aramid fiber precursor after winding, drying, wherein, described coagulating bath is sulfuric acid solution, be made up of sulfuric acid and water, the mass fraction of sulfuric acid is 2.0%-15.0%, and the temperature of coagulating bath is 1-12 DEG C.
Preferably, the height of the air layer between described coagulating bath and spinnerets is 3-15mm.
Preferably, described from the time of staying of liquid stream coagulating bath that spinnerets is extruded be 1.5-4.8s.
Preferably, described PPTA-H
2sO
4the preparation method of spinning solution is: the concentrated sulfuric acid and fuming sulphuric acid are mixed to get mass fraction 99.5% ~ 100% sulfuric acid, cooling curing at-5 ~-12 DEG C, then blended at-5 ~-12 DEG C with PPTA resin, obtain PPTA-H
2sO
4blend, wherein the mass fraction of PPTA is 16 ~ 22%, blend is obtained PPTA liquid crystal solution through the twin-screw mixed dissolution of 80 ~ 105 DEG C, through deaeration, obtains PPTA-H after filtration
2sO
4spinning solution.
Preferably, described washing comprises washing, alkali cleaning, washing three grades washing successively.First order washing is used for except desolventizing and impurity, second level washing for removing acid impurities, third level washing with the impurity do not eliminated.
More preferably, described washing adopts deionized water, and the alkali that alkali cleaning adopts is weak base, and the mass fraction of alkali lye is 0.5-5.0%.
More preferably, the alkali that described alkali cleaning adopts is calcium hydroxide, sodium carbonate, sodium bicarbonate, saleratus or ammoniacal liquor.
Preferably, described baking temperature is 100 DEG C-150 DEG C.
Preferably, described coagulating bath is incubated by low-temperature cooling fluid circulating pump.
Double diffusion process between the stoste thread extruded from spinnerets in coagulation forming method of the present invention and coagulating bath, in coagulating bath, the concentration of sulfuric acid will have a strong impact on double diffusion process, sulfuric acid concentration is too high, double diffusion is slow, as-spun fibre surface forms compacted zone, be unfavorable for the diffusion of fibrous inside sulfuric acid, will the compactness of fibrous inner structure be had a strong impact on.Coagulation bath temperature, in lower scope, is 1-12 DEG C.Due in dry spray-wet spinning, spinning solution from spinnerets out after keep liquid crystal state structure, after air section, enter coagulating bath rapidly, low temperature coagulating bath is conducive to freezing of liquid crystal aligning structure in thread, thus is conducive to the preparation of high-strength high-modulus fibre; On the other hand, the double diffusion between thread and coagulating bath can be accelerated with the raising of coagulation bath temperature, thus upsets orientation texture, makes strand inside form micropore, affects the mechanical property of fiber.The height of the air layer in the present invention between coagulating bath and spinnerets is 3-15mm.Excessive height, spinning head may produce doubling or fracture of wire at air section, highly too low, makes the solvent evaporates in spinning solution thread slow, cannot form film on thread surface, thus makes its double diffusion in coagulating bath violent, makes fibrous inside form micropore.
Compared with prior art, the invention has the beneficial effects as follows:
(1) adopt the present invention, this extraordinary coagulating bath can significantly improve the production efficiency of p-aramid fiber, reduces the production cost of fiber.Experiment prove, this coagulating bath parameters be arranged so that stoste thread fully can be frozen into as-spun fibre in the time shorter in coagulating bath, the speed of production of p-aramid fiber spinning is at least improved 2 times.
(2) coagulating bath of the present invention adopts the sulfuric acid solution of low concentration, can improve the concentration difference between solvent and spinning solution thread, accelerates diffusion, improves freezing rate, guarantees that fiber fully solidifies in coagulating bath, improve again the production efficiency of fiber.
(3) the present invention adopts low temperature to solidify, low temperature can inhibit diffusion velocity on the one hand, makes the fine densification of fibre structure, on the other hand, low temperature coagulating bath is conducive to freezing of liquid crystal aligning structure in thread, thus is conducive to the preparation of high-strength and high-modulus p-aramid fiber.
(4) fiber of the present invention comes out to the air section of coagulating bath through appropriate height from spinning head.Air section is conducive to the stretching of spinning solution, and spinning solution is height-oriented through spinneret orifice, and air section, to spinnerets insulation, maintains the liquid crystal state state structure of spinning solution, thus makes as-spun fibre have higher shower nozzle draw ratio.
(5) coagulation bath condition of the present invention can significantly fall low-fiber fiber number, improve the intensity of para-aramid fiber, and the visual defects of fiber can be reduced, improve fiber quality, thus effectively improve the stability of spinning technique and the quality of fiber product.
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
Dry-wet spinning prepares a solidification forming method for p-aramid fiber, and concrete steps are:
The concentrated sulfuric acid (AR level, concentration (95-98) %, Kunshan Jingke Micro-Electronics Material Co.. Ltd.) and fuming sulphuric acid (are analyzed pure, SO
3mass fraction is 50%, Shanghai development chemical reagent two factory), by be mixed to get mass fraction 99.5% ~ 100% the concentrated sulfuric acid, cooling curing under-10 DEG C of environment, then with PPTA resin (η
inh=5.8dL/g, Hebei Guigu Chemical Co., Ltd)-10 DEG C of low temperature are blended, obtain PPTA-H
2sO
4blend, wherein the mass fraction of PPTA is 18.5%, blend is obtained PPTA liquid crystal solution through the twin-screw mixed dissolution of 90 DEG C, through deaeration, obtains PPTA-H after filtration
2sO
4spinning solution.
By PPTA-H
2sO
4spinning solution is extruded from spinnerets, and on spinnerets, the aperture of spinneret orifice is 0.07mm, by the liquid stream extruded from spinnerets vertically through air layer, enter in coagulating bath, drawn by godet roller, obtain as-spun fibre, through washing, alkali cleaning, washing, winding, para-aramid fiber precursor is obtained after 100 DEG C of dryings, wherein, described coagulating bath is sulfuric acid solution, is made up of sulfuric acid and water, the mass fraction of sulfuric acid is 6.0%, and the temperature of coagulating bath is 1 DEG C.The height of the air layer between described coagulating bath and spinnerets is 5mm.Described from the time of staying of liquid stream coagulating bath that spinnerets is extruded be 1.5s.Described washing adopts deionized water, and the alkali that alkali cleaning adopts is sodium carbonate, and its mass fraction is 4.5%.Described coagulating bath is incubated by low-temperature cooling fluid circulating pump.
Tested by fibrous mechanical property, the intensity of the p-aramid fiber precursor of the present embodiment gained is 24.82cN/dtex, compared to domestic p-aramid fiber precursor, intensity increases by 7.03%, tested by X-ray diffraction, the degree of crystallinity of the p-aramid fiber precursor of the present embodiment gained increases by 3%, and the degree of orientation increases by 0.3%.
Embodiment 2
Dry-wet spinning prepares a solidification forming method for p-aramid fiber, and concrete steps are:
The concentrated sulfuric acid (AR level, concentration (95-98) %, Kunshan Jingke Micro-Electronics Material Co.. Ltd.) and fuming sulphuric acid (are analyzed pure, SO
3mass fraction is 50%, Shanghai development chemical reagent two factory), by be mixed to get mass fraction 99.5% ~ 100% the concentrated sulfuric acid, cooling curing under-12 DEG C of environment, then with PPTA resin (η
inh=5.8dL/g, Hebei Guigu Chemical Co., Ltd) blended at-12 DEG C of low temperature, obtain PPTA-H
2sO
4blend, wherein the mass fraction of PPTA is 18.5%, blend is obtained PPTA liquid crystal solution through the twin-screw mixed dissolution of 90 DEG C, through deaeration, obtains PPTA-H after filtration
2sO
4spinning solution.
By PPTA-H
2sO
4spinning solution is extruded from spinnerets, and on spinnerets, the aperture of spinneret orifice is 0.07mm, by the liquid stream extruded from spinnerets vertically through air layer, enter in coagulating bath, drawn by godet roller, obtain as-spun fibre, through washing, alkali cleaning, washing, winding, para-aramid fiber precursor is obtained after 120 DEG C of dryings, wherein, described coagulating bath is sulfuric acid solution, is made up of sulfuric acid and water, its mass fraction is 3.0%, and the temperature of coagulating bath is 6 DEG C.The height of the air layer between described coagulating bath and spinnerets is 5mm.Described from the time of staying of liquid stream coagulating bath that spinnerets is extruded be 2.0s.Described washing adopts deionized water, and the alkali that alkali cleaning adopts is saleratus, and its mass fraction is 3.5%.Described coagulating bath is incubated by low-temperature cooling fluid circulating pump.
Tested by fibrous mechanical property, the intensity of the p-aramid fiber precursor of the present embodiment gained is 24.66cN/dtex, compared to domestic p-aramid fiber precursor, intensity increases by 6.34%, tested by X-ray diffraction, the p-aramid fiber precursor degree of crystallinity of the present embodiment gained increases by 2%, and the degree of orientation increases by 0.2%.
Embodiment 3
Dry-wet spinning prepares a solidification forming method for p-aramid fiber, and concrete steps are:
The concentrated sulfuric acid (AR level, concentration (95-98) %, Kunshan Jingke Micro-Electronics Material Co.. Ltd.) and fuming sulphuric acid (are analyzed pure, SO
3mass fraction is 50%, Shanghai development chemical reagent two factory), by be mixed to get mass fraction 99.5% ~ 100% the concentrated sulfuric acid, cooling curing under-11 DEG C of environment, then with PPTA resin (η
inh=5.8dL/g, Hebei Guigu Chemical Co., Ltd) blended under-11 DEG C of environment, obtain PPTA-H
2sO
4blend, wherein the mass fraction of PPTA is 18.5%, blend is obtained PPTA liquid crystal solution through the twin-screw mixed dissolution of 90 DEG C, through deaeration, obtains PPTA-H after filtration
2sO
4spinning solution.
By PPTA-H
2sO
4spinning solution is extruded from spinnerets, the aperture 0.07mm of spinneret orifice on spinnerets, by the liquid stream extruded from spinnerets vertically through air layer, enter in coagulating bath, drawn by godet roller, obtain as-spun fibre, through washing, alkali cleaning, washing, winding, para-aramid fiber precursor is obtained after 130 DEG C of dryings, wherein, described coagulating bath is sulfuric acid solution, is made up of sulfuric acid and water, its mass fraction is 7.0%, and the temperature of coagulating bath is 3 DEG C.The height of the air layer between described coagulating bath and spinnerets is 8.5mm.Described from the time of staying of liquid stream coagulating bath that spinnerets is extruded be 3.0s.Described washing adopts deionized water, and the alkali that alkali cleaning adopts is sodium carbonate, and its mass fraction is 3.0%.Described coagulating bath is incubated by low-temperature cooling fluid circulating pump.
Tested by fibrous mechanical property, the intensity of the p-aramid fiber precursor of the present embodiment gained is 24.44cN/dtex, compared to domestic p-aramid fiber precursor, intensity increases by 15%, tested by X-ray diffraction, the p-aramid fiber precursor degree of crystallinity of the present embodiment gained increases by 1.2%, and the degree of orientation increases by 0.15%.
Embodiment 4
Dry-wet spinning prepares a solidification forming method for p-aramid fiber, and concrete steps are:
The concentrated sulfuric acid (AR level, concentration (95-98) %, Kunshan Jingke Micro-Electronics Material Co.. Ltd.) and fuming sulphuric acid (are analyzed pure, SO
3mass fraction is 50%, Shanghai development chemical reagent two factory), by be mixed to get mass fraction 99.5% ~ 100% the concentrated sulfuric acid, cooling curing under-8 DEG C of environment, then with PPTA resin (η
inh=5.8dL/g, Hebei Guigu Chemical Co., Ltd) blended under-8 DEG C of environment, obtain PPTA-H
2sO
4blend, wherein the mass fraction of PPTA is 18.5%, blend is obtained PPTA liquid crystal solution through the twin-screw mixed dissolution of 90 DEG C, through deaeration, obtains PPTA-H after filtration
2sO
4spinning solution.
By PPTA-H
2sO
4spinning solution is extruded from spinnerets, and on spinnerets, the aperture of spinneret orifice is 0.07mm, by the liquid stream extruded from spinnerets vertically through air layer, enter in coagulating bath, drawn by godet roller, obtain as-spun fibre, through washing, alkali cleaning, washing, winding, para-aramid fiber precursor is obtained after 110 DEG C of dryings, wherein, described coagulating bath is sulfuric acid solution, is made up of sulfuric acid and water, its mass fraction is 13.0%, and the temperature of coagulating bath is 11 DEG C.The height of the air layer between described coagulating bath and spinnerets is 12mm.Described from the time of staying of liquid stream coagulating bath that spinnerets is extruded be 4.5s.Described washing adopts deionized water, and the alkali that alkali cleaning adopts is calcium hydroxide, and its mass fraction is 1.0%.Described coagulating bath is incubated by low-temperature cooling fluid circulating pump.
Tested by fibrous mechanical property, the intensity of the p-aramid fiber precursor of the present embodiment gained is 24.44cN/dtex, compared to domestic p-aramid fiber precursor, intensity increases by 4.14%, tested by X-ray diffraction, the p-aramid fiber precursor degree of crystallinity of the present embodiment gained increases by 0.8%, and the degree of orientation increases by 0.1%.
Embodiment 5
Dry-wet spinning prepares a solidification forming method for p-aramid fiber, and concrete steps are:
The concentrated sulfuric acid (AR level, concentration (95-98) %, Kunshan Jingke Micro-Electronics Material Co.. Ltd.) and fuming sulphuric acid (are analyzed pure, SO
3mass fraction is 50%, Shanghai development chemical reagent two factory), by be mixed to get mass fraction 99.5% ~ 100% the concentrated sulfuric acid, cooling curing under-5 DEG C of environment, then with PPTA resin (η
inh=5.8dL/g, Hebei Guigu Chemical Co., Ltd) blended under-5 DEG C of environment, obtain PPTA-H
2sO
4blend, wherein the mass fraction of PPTA is 18.5%, blend is obtained PPTA liquid crystal solution through the twin-screw mixed dissolution of 90 DEG C, through deaeration, obtains PPTA-H after filtration
2sO
4spinning solution.
By PPTA-H
2sO
4spinning solution is extruded from spinnerets, and on spinnerets, the aperture of spinneret orifice is 0.07mm, by the liquid stream extruded from spinnerets vertically through air layer, enter in coagulating bath, drawn by godet roller, obtain as-spun fibre, through washing, alkali cleaning, washing, winding, para-aramid fiber precursor is obtained after 150 DEG C of dryings, wherein, described coagulating bath is sulfuric acid solution, is made up of sulfuric acid and water, the mass fraction of sulfuric acid is 15.0%, and the temperature of coagulating bath is 12 DEG C.The height of the air layer between described coagulating bath and spinnerets is 15mm.Described from the time of staying of liquid stream coagulating bath that spinnerets is extruded be 4.8s.Described washing adopts deionized water, and the alkali that alkali cleaning adopts is sodium bicarbonate, and its mass fraction is 4.0%.Described coagulating bath is incubated by low-temperature cooling fluid circulating pump.
Tested by fibrous mechanical property, the intensity of the p-aramid fiber precursor of the present embodiment gained is 23.9cN/dtex, compared to domestic p-aramid fiber precursor, intensity increases by 3.06%, tested by X-ray diffraction, the p-aramid fiber precursor degree of crystallinity of the present embodiment gained increases by 0.4%, and the degree of orientation increases by 0.07%.
Claims (9)
1. dry-wet spinning prepares a solidification forming method for p-aramid fiber, and it is characterized in that, concrete steps comprise: by PPTA-H
2sO
4spinning solution is extruded from spinnerets, by the liquid stream extruded from spinnerets vertically through air layer, enter in coagulating bath, drawn by godet roller, obtain as-spun fibre, through washing, obtain para-aramid fiber precursor after winding, drying, wherein, described coagulating bath is sulfuric acid solution, be made up of sulfuric acid and water, its mass fraction is 2.0%-15.0%, and the temperature of coagulating bath is 1-12 DEG C.
2. dry-wet spinning as claimed in claim 1 prepares the solidification forming method of p-aramid fiber, and it is characterized in that, the height of the air layer between described coagulating bath and spinnerets is 5-15mm.
3. dry-wet spinning as claimed in claim 1 prepares the solidification forming method of p-aramid fiber, it is characterized in that, described from the time of staying of liquid stream coagulating bath that spinnerets is extruded be 1.5-4.8s.
4. dry-wet spinning as claimed in claim 1 prepares the solidification forming method of p-aramid fiber, it is characterized in that, described PPTA-H
2sO
4the preparation method of spinning solution is: the concentrated sulfuric acid and fuming sulphuric acid are mixed to get mass fraction 99.5% ~ 100% sulfuric acid, cooling curing at-5 ~-12 DEG C, then blended at-5 ~-12 DEG C with PPTA resin, obtain PPTA-H
2sO
4blend, wherein the mass fraction of PPTA is 16 ~ 22%, blend is obtained PPTA liquid crystal solution through the twin-screw mixed dissolution of 80 ~ 105 DEG C, through deaeration, obtains PPTA-H after filtration
2sO
4spinning solution.
5. dry-wet spinning as claimed in claim 1 prepares the solidification forming method of p-aramid fiber, and it is characterized in that, described washing comprises washing, alkali cleaning, washing three grades washing successively.
6. dry-wet spinning as claimed in claim 5 prepares the solidification forming method of p-aramid fiber, it is characterized in that, described washing adopts deionized water, and the alkali that alkali cleaning adopts is weak base, and its mass fraction is 0.5-5.0%.
7. dry-wet spinning as claimed in claim 6 prepares the solidification forming method of p-aramid fiber, it is characterized in that, the alkali that described alkali cleaning adopts is calcium hydroxide, sodium carbonate, sodium bicarbonate, saleratus or ammoniacal liquor.
8. dry-wet spinning as claimed in claim 1 prepares the solidification forming method of p-aramid fiber, and it is characterized in that, described baking temperature is 100 DEG C-150 DEG C.
9. dry-wet spinning as claimed in claim 1 prepares the solidification forming method of p-aramid fiber, and it is characterized in that, described coagulating bath is incubated by low-temperature cooling fluid circulating pump.
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