CN101514495A - Method for producing dope-dyeing metaposition aramid fibers by adopting technique of infusion before spinning - Google Patents

Method for producing dope-dyeing metaposition aramid fibers by adopting technique of infusion before spinning Download PDF

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Publication number
CN101514495A
CN101514495A CNA2008101464192A CN200810146419A CN101514495A CN 101514495 A CN101514495 A CN 101514495A CN A2008101464192 A CNA2008101464192 A CN A2008101464192A CN 200810146419 A CN200810146419 A CN 200810146419A CN 101514495 A CN101514495 A CN 101514495A
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meta
stoste
spun
aramid
color paste
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吴学东
陈惠敏
吴林才
付家明
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SHANGHAI SHILIN FIBER MATERIAL CO Ltd
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SHANGHAI SHILIN FIBER MATERIAL CO Ltd
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Abstract

The invention relates to a method for producing dope-dyeing metaposition aramid fibers by adopting a technique of infusion before spinning. A system for the infusion before spinning is arranged at a position abutting against a silk-spinning machine and comprises a metaposition aramid fiber stock solution metering pump, a pigment color paste metering pump, a mixer, a pressure balancer and a pressure self-control system, wherein the mixer is a first-stage mixer, or a first-stage mixer and a second-stage mixer which are connected in series sequentially; a metaposition aramid fiber stock solution and a pigment color paste are metered after on-line continuous filtration and deaeration, and then are dispersed and mixed in the mixer; and a coloration stock solution after mixing is conveyed to the silk-spinning machine for spinning after passing through the pressure balancer. The method ensures that the added pigment color paste and the stock solution are dispersed and mixed evenly, the prior devices and the prior process on the production line are unnecessary to be adjusted specially, the pipeline from a mixing position to a spinning position is short, the transitional batch is less, the pipeline is convenient to clean, and the down time is short. With the method, the pigment addition required to achieve the same fiber color depth is less.

Description

Injection technique was made the method for spun dyeing meta-aramid fiber before employing was spun
Technical field
The invention belongs to the blending and modifying field of Chemical Engineering, meta-aramid fibers manufacturing technique, polymer, injection technique was made the method for spun dyeing meta-aramid fiber before especially a kind of employing was spun.
Prior art
From nineteen sixty for E.I.Du Pont Company's invention meta-aramid fibers since, its technology has been compared open fully, United States Patent (USP) 2708617,3006899,3063966,3232910,3240760,3287324,3354125,3360598,3376268,3376269,3414645,3627737,3640970,4073837, Chinese patent ZL97194871.2, ZL00804010.9, ZL03116187.1, CN1974892A and Japanese patent application publication No. 8-74121,8-74122,10-53920,10-88421,35-14399,47-10863,48-4661,48-17551,49-129096 etc. all relate to stoste preparation and spining technology wherein.Summary is got up, and the polymerization of meta-aromatic polyamide comprises low temperature solution polymerization and interfacial polymerization, and spinning process comprises dry method, wet method and dried/wet method etc.
For overcoming the dyeing difficult problem of meta-aramid fibers, many years ago, Du Pont and Supreme Being people company directly add pigment to and carry out spinning in the meta-aromatic polyamide stoste, and the spun dyeing meta-aramid fiber is made in the beginning commercialization.But there is not concrete technology open.
CN1847475A discloses a kind of manufacture method of spun dyeing meta-aramid fiber, operation such as technological process comprises that stoste preparation, mill base preparation, stoste are mixed with mill base, spinning and post processing, but the mixed method of stoste and mill base is not related to.
To mixing of stoste and mill base, chemical fibre industry technical staff's technique known scheme is, in the stoste preparation process or finish the back in the stoste preparation and mix with mill base employing slurry formula stirring means and disperse, process in batches, discontinuous.
CN1740412A discloses a kind of solvent spinning on-line continuous metering to be added and mixed method, it is the so-called preceding injection technique of spinning, it is to increase by devices such as cover online metering interpolation, mixing and pressure balance near the spinning machine position, constitute one and complete spin preceding injected system, this technology has been successfully applied to the manufacturing of original liquid coloring fiber on large-scale viscose glue and acrylic fiber production process line, reached even dispersion and the effect of mixing.
Do not spin the report that preceding injection technique is applied to the manufacturing of spun dyeing meta-aramid fiber but have as yet at present.
Applicant of the present invention finds that behind big quantity research in the manufacture method of spun dyeing meta-aramid fiber, the mixed method of stoste and dispersible pigment color paste is crucial.
If adopt and starch the formula stirring mixing method in batches, the problem of existence is: at first starch the formula stirring theory and determined that pigment fine particle and high viscosity stoste are difficult to guarantee all even effective dispersion and mix, will influence spinning process and carry out smoothly and fiber quality; The 2nd, the residing stoste vehicle headway of hybrid position spinning machine is far away, and pipeline is long, and the transition when causing variety renovation is criticized oversize, and line clear difficulty, down time are long, must enough could offset these negative effects greatly in batches; The 3rd, because the original liquid coloring interpolation is granules of pigments, must do bigger adjustment to the technologies such as filtration on the flow process; The 4th, in case dispersion and mixed effect are not good, will cause the waste of large quantities of raw materials and influence to produce.
Summary of the invention
Based on the existing in prior technology problem, require manufacture method that exploitation makes new advances with the economy that solves fiber and make, in batches, the problem of aspects such as production line adaptability and product quality.The method must satisfy spin before on-line metering add, simple, the stable accurate and maintaining of evenly dispersions/mixings, the system requirement of aspect such as conveniently, and as often as possible selection standard or ripe unit be so that system cost is lower, and can adapt to requirements dissimilar and that the different proportion dispersible pigment color paste adds.Before carrying out online spinning, inject and mix near the position of spinning machine, and guarantee that dispersible pigment color paste evenly mixes and disperses, do not produce additional bubbles, need not adjust specially equipment on the production line and technology with stoste, make hybrid position short to the pipeline of spinning machine, transition is criticized few, line clear is convenient, and down time is short.Basic goal of the present invention is to have minimum production cost and best properties of product for the spun dyeing meta-aramid fiber that guarantees manufacturing, the demand that adapts to the market small lot provides a kind of employing to spin the method that preceding injection technique is made the spun dyeing meta-aramid fiber.
Another technical problem to be solved by this invention is to provide a kind of meta-aramid fibers product that adopts above-mentioned preparation method to obtain.
The present invention solves the problems of the technologies described above the technical scheme of being taked: injection technique was made the method for spun dyeing meta-aramid fiber before a kind of employing was spun, spin preceding injected system in position setting near spinning machine, injected system comprised meta-aramid stoste measuring pump before this spun, the dispersible pigment color paste measuring pump, blender, pressurizer and pressure automatic control system, wherein, blender is an one-level blender, or two one-level blender and secondary blenders of connecting in regular turn, on-line continuous constantly will be through filtering and after the meta-aramid stoste of deaeration and dispersible pigment color paste measure, send into blender together and disperse fully and mix, mixed painted stoste is carried out spinning through being delivered to spinning machine behind the pressurizer.
The inventive method can satisfy the requirement of spun dyeing meta-aramid fiber manufacturing to the stability and the precision of on-line mixing, according to material proterties and mixing requirement, blender can be provided with two of series connection in regular turn, and promptly one-level blender, secondary blender also can only only adopt the one-level blender.
Concrete, the filtration of meta-aramid stoste process, deaeration are after measuring pump delivers into the one-level blender, the one-level blender is sent in metering after filtration of dispersible pigment color paste process and the deaeration, two kinds of components carry out preliminary dispersion and mixing at this, and then enter the secondary blender and carry out further meticulous dispersion and mixing, enter pressurizer through the painted stoste of mixing and carry out equalizing pressure, and be transported to spinning machine thus and carry out spinning.At the pressurizer place, the pressure and the liquid level of spinning solution detected, and in view of the above meta-aramid stoste measuring pump and dispersible pigment color paste measuring pump are carried out the flow adjustment, make the pressure of painted stoste in the pressurizer and liquid level keep stable.Wherein, controller adopts PLA control, the place changes into the signal of telecommunication by pressure transmitter with pressure signal at pressurizer, and the PLA controller is regulated the frequency converter of measuring pump according to this signal and liquid level signal according to certain algorithm, adjusts the flow of measuring pump by regulating the measuring pump motor rotary speed.
On the basis of such scheme, the measuring pump described in the injected system adopts a kind of in gear wheel metering pump, diaphragm metering pump, plunger metering pump, the screw pump (comprising the anti-NEMO of speeding single-screw (single screw) pump) before spinning.The measuring accuracy of injected system is the stack of meta-aramid stoste measuring pump and the two precision of dispersible pigment color paste measuring pump before spinning.
On the basis of such scheme, the one-level blender described in the injected system is static mixer or rotor/stator high-shear mixer before spinning, and described secondary blender is static mixer or rotor/stator high-shear mixer.
The one-level blender can be static mixer or rotor/stator high-shear mixer.The secondary blender also can be static mixer or rotor/stator high-shear mixer.Wherein, static mixer is big fluid streams is divided into little fluid streams and mixes mutually, and dispersion/mixed effect depends on to be cut apart fineness and cut apart/hybrid frequency.The rotor/stator high-shear mixer is by the circumferential trickle slot of rotor/stator fluid to be cut into small unit and mix mutually by the high shear force that rotor/stator rotates generation at a high speed.The effect of disperseing and mixing depends on the cell size and the cutting/hybrid frequency of being cut, and the unit that cuts into is more little, the frequency of cutting/mixing is high more, and dispersion and the effect of mixing are just good more.The rotor/stator high-shear mixer also has the effect that granules of pigments in the mill base is pulverized.
The rotor/stator high-shear mixer is made up of stator, rotor, axle, cavity (containing cooling jacket), import and export and motor.Its architectural feature is: rotor and stator all are cylindrical structures, i.e. a side opening, opposite side sealing, have axial groove on circumferential wall, this groove can be an enclosed slot, also can be open slot, if open slot, opening direction is consistent with rotor and stator cylinder opening direction.Stator and rotor coaxial are installed, and rotor is placed among the stator, between gapped, constitute one group of complete stator rotor structure, stator rotor is installed in the cavity, cavity is provided with the heating and cooling chuck, can feed heating agent or refrigerant and heat or cool off.The in succession axial inlet of blender of stator rotor openend, at the other end, the stator rotor axle links to each other with motor by the axle envelope, axle seal and stator rotor between be provided with the radially outlet of blender.Its course of work is: rotor is high speed rotary under the driving of motor, material is axially sucked at the high speed rotary of import owing to rotor, under the rotor action of centrifugal force, material is radially dished out at a high speed, in the slotted eye of rotor and stator,, realize pulverizing and disperseing, and rebound at cavity inner wall by high speed shear, finish further immixture, discharge material through outlet at last.One-level, secondary, three grades even multi-stage rotor/stator can be installed in cavity, and every grade of groove width can be consistent, also can progressively reduce, and makes pulverizing, dispersion and mixed effect meticulous step by step.Further, except that can adopting a pair of rotor/stator configuration, each grade can also adopt two pairs of rotor/stators to form the rotor-stator-rotor-stator four-layer structure of layering from the inside to the outside, perhaps adopt three pairs of rotor/stators to form the rotor-stator-rotor-stator of layering from the inside to the outside-six layers of structure of rotor-stator, form meticulousr dispersion, mixing and pulverization.
On the basis of such scheme, the pressurizer described in the injected system comprises painted stoste import, the outlet of painted stoste, compressed air import and export, manometer, pressure transmitter and liquid level gauge before spinning, painted stoste import is connected with the outlet of blender, and outlet is connected with spinning machine.
Described pressurizer is a sealed pressure vessel, painted stoste is carried out pressure balance at this, be sealed with compressed air in the pressurizer, the pressure of painted stoste is relevant with air pressure wherein and liquid level, can it be compensated and balance by the Flow-rate adjustment of meta-aramid stoste and dispersible pigment color paste.Flow-rate adjustment is specifically finished by a closed loop robot control system(RCS), this robot control system(RCS) detected pressures balancer inner air pressure and painted stoste liquid level, and corresponding adjusting meta-aramid stoste and dispersible pigment color paste measuring pump flow, make that painted stoste pressure stability keeps the proportions constant of meta-aramid stoste and dispersible pigment color paste constant at certain level simultaneously in the pressurizer.Described robot control system(RCS) comprises PLA and corresponding software, pressure transmitter, liquid level gauge, measuring pump motor and frequency converter etc., by pressure and the liquid level in pressure transmitter and the liquid level gauge difference detected pressures balancer, input PLA, regulate the rotating speed of metering pump motor by frequency converter according to algorithm, and then the flow of adjusting meta-aramid stoste and dispersible pigment color paste measuring pump, make the air pressure in the pressurizer keep stable, thereby the pressure that makes the painted stoste of output keeps stable, and keeps stoste and dispersible pigment color paste proportions constant.
On the basis of such scheme, described meta-aramid stoste is 1: 0.0002~0.5000 with the mixing quality ratio of dispersible pigment color paste.
The mass ratio of meta-aramid stoste and dispersible pigment color paste is specifically as follows 1: 0.0002, and 0.0010,0.0050,0.0100,0.0500,0.1000,0.2000,0.3000,0.4000 or 0.5000.
On the basis of such scheme, in the described meta-aramid stoste, the mass concentration of poly is 5~25%, and dicyandiamide solution is dimethylacetylamide/calcium chloride system (DMAc/CaCl 2), DMAc/CaCl 2CaCl in the dicyandiamide solution 2Mass concentration≤3% is low salt system and CaCl 2Mass concentration>3% is high salt system, CaCl 2Mass concentration the highest by 18%, generally be not higher than 10% and be advisable, poly is by the preparation of low temperature solution polymerization method or interfacial polymerization.
Concrete stoste technology of preparing is with reference to related known and public technology, as United States Patent (USP) 2708617,3006899,3063966,3232910,3240760,3287324,3354125,3376268,3376269 and Chinese patent ZL00804010.9, ZL03116187.1, CN1974892A and Japanese patent application publication No. 35-14399,47-10863,48-4661,49-129096 etc.
On the basis of such scheme, a kind of prescription of dispersible pigment color paste is provided, described dispersible pigment color paste is the dispersion liquid of granules of pigments in solvent, and solvent is dimethylacetylamide or dimethylacetylamide/calcium chloride system, and dispersible pigment color paste comprises following component by weight percentage:
Pigment 5~25%
Dispersant 1~6%
Auxiliary agent 0.01~1.00%
Calcium chloride 0~9%
Dimethylacetylamide 59~93.99%
Wherein, the granules of pigments particle diameter is less than 1 μ m, and pigment is one or more the combination in azo class, many lopps, the condensed ring class mineral-type pigment.
The consumption of concrete pigment can be 5,8,10,12,15,18,20,22 or 25%;
The consumption of dispersant can be 1,2,3,4,5 or 6%;
The consumption of auxiliary agent can be 0.01,0.05,0.1,0.2,0.5,0.8 or 1.0%;
The consumption of calcium chloride can be 0,1,2,3,5,6,8 or 9%;
The consumption of dimethylacetylamide can be 59,60,65,70,75,80,85,90,92 or 93.99%.
On the basis of such scheme, the prescription of another kind of dispersible pigment color paste is provided, described dispersible pigment color paste is the dispersion liquid of granules of pigments in meta-aramid stoste dilution, dilution is identical with solvent in the stoste with solvent, promptly, solvent with stoste further dilutes stoste, adds granules of pigments again and disperse to make dispersible pigment color paste, and dispersible pigment color paste comprises following component by weight percentage:
Pigment 5~25%
Poly 0.1~25.0%
Calcium chloride 0.1~9.0%
Dimethylacetylamide 41~94.8%,
Wherein, the granules of pigments particle diameter is less than 1 μ m, and pigment is one or more the combination in azo class, many lopps, the condensed ring class mineral-type pigment.
The consumption of concrete pigment can be 5,8,10,12,15,18,20,22 or 25%;
The consumption of poly can be 0.1,0.5,1,5,10,15,20 or 25%;
The consumption of calcium chloride can be 0.1,0.5,1.0,2.0,3.0,5.0,6.0,8.0 or 9.0%;
The consumption of dimethylacetylamide can be 41,42,45,50,55,60,65,70,75,80,85,90,92 or 94.8%.
Described spinning process comprises dry method, wet method and does/wet method.Known and the public technology that concrete spining technology is made with reference to meta-aramid fibers is as United States Patent (USP) 3360598,3414645,3627737,3640970,4073837 and Chinese patent ZL97194871.2, ZL00804010.9, ZL200510026893.8 and Japanese patent application publication No. 8-74121,8-74122,10-53920,10-88421,35-14399,48-17551 etc.
Spin the prepared meta-aramid fibers product of method that preceding injection technique is made the spun dyeing meta-aramid fiber at above-mentioned employing, wherein, in the described painted meta-aramid fibers, the mass percent of pigment is 0.01~10.00%.Pigment particle in fiber is thinner, be more evenly distributed the characteristics that quality is more excellent, production cost is lower.
The invention has the beneficial effects as follows:
The present invention can adapt to spun dyeing meta-aramid fiberline small lot flexible manufacturing requirement, and this system can adapt to the requirement of dissimilar dispersible pigment color pastes and adding proportion.Because the interpolation of mill base and stoste and hybrid position are near spinning machine, and static mixer and rotor/stator high-shear mixer have been adopted, can guarantee that the dispersible pigment color paste that adds evenly disperses with stoste and mixes, need not adjust specially existing equipment on the production line and technology, hybrid position is short to the pipeline of spinning station, transition is criticized few, line clear is convenient, and down time is short.In addition,, can further reduce the particle diameter of pigment and improve uniformity, spinning process and fiber quality are had active influence because the rotor/stator high-shear mixer has pulverization to granules of pigments.The original liquid coloring fiber is carried out microscope and electron microscopic observation discovery, granules of pigments fineness in the fiber evenly, be uniformly dispersed, and, fiber also finds by being carried out strength test, spun dyeing meta-aramid fiber that injection technique was made before employing was spun and not coloured fiber comparison accordingly, its fibre strength does not descend or descends few, verified that further the granules of pigments fineness is thinner in the fiber of making by injection technique before spinning, more all even dispersion is better, made cooperative effect between granules of pigments and the poly greater than its impurity effect.And, because injected system makes pigment particle size thinner to the pulverization of pigment before spinning, therefore, reach same fiber color color depth, needed pigment addition will reduce.Therefore, lower, the better quality of spun dyeing meta-aramid fiber cost of the present invention's manufacturing.In addition, because it all is mature technique that device that each unit of system is adopted or equipment are still used in principle, so system is simple, stable, accurate, reliable, cost is low, and maintaining is convenient, adapts to the application requirements that the spun dyeing meta-aramid fiber is made.
Description of drawings
Fig. 1 is a process chart of the present invention.
The specific embodiment
Embodiment 1
See also Fig. 1 for shown in the process chart of the present invention, spin preceding injected system in position setting near spinning machine, injected system comprised meta-aramid stoste measuring pump before this spun, the dispersible pigment color paste measuring pump, blender, pressurizer and pressure automatic control system, wherein, blender is two the one-level blender and the secondary blenders of series connection in regular turn, after on-line continuous ground will measure through the meta-aramid stoste of filtration and deaeration and dispersible pigment color paste, send into one-level blender and secondary blender together in regular turn and disperse and mix, mixed painted stoste is carried out spinning through being delivered to spinning machine behind the pressurizer.
To produce that 300 kilograms of spun dyeing meta-aramid fiberlines are supporting to spin preceding injected system daily, meta-aramid stoste measuring pump adopts 80 liters of/hour gear wheel metering pumps, dispersible pigment color paste adopts 5 liters of/hour diaphragm metering pumps, the one-level blender adopts 90 liters of/hour static mixers, the secondary blender adopts 90 liters of/hour rotor/stator high-shear mixers, and the fiber production ability of corresponding spinning machine is 300 kilograms/day.
Embodiment 2
To produce that 1000 kilograms of spun dyeing meta-aramid fiberlines are supporting to spin preceding injected system daily.Meta-aramid stoste measuring pump adopts 260 liters of/hour anti-speeding (NEMO) single-screw (single screw) pump, dispersible pigment color paste adopts 16 liters of/hour plunger metering pumps, the one-level blender adopts 280 liters of/hour static mixers, the secondary blender adopts 280 liters of/hour rotor/stator high-shear mixers, and the fiber production ability of corresponding spinning machine is 1000 kilograms/day.
Embodiment 3
Injection technique was made original liquid coloring black meta-aramid fibers before employing was spun.
In the meta-aramid stoste, poly concentration is 20wt%, and dicyandiamide solution is DMAc/CaCl 2, CaCl wherein 2Concentration is 3wt%;
In the dispersible pigment color paste, carbon black content is 20wt%, and dispersant is 5wt%, and auxiliary agent content is 0.1wt%, and surplus is solvent DMAc, and carbon black granules is less than 1 μ m.
Adopt the preceding injected system of spinning of embodiment 1 or 2, regulate stoste and mill base measuring pump flow and guarantee that the carbon black ratio is 4.0wt% in the fiber, above-mentioned painted stoste is carried out wet spinning.Coagulation forming in 20 ℃ spinning bath, spinning bath consists of: 35wt%DMAc, 20wt% calcium chloride and 45wt% water, again by stretching, washing, oven dry, heat treatment, curl and cut-out, packing etc. become original liquid coloring black meta-aramid finished fiber.
Embodiment 4
Injection technique was made original liquid coloring navy meta-aramid fibers before employing was spun.
In the meta-aramid stoste, the poly weight concentration is 18%, and dicyandiamide solution is DMAc/CaCl 2, CaCl wherein 2Concentration is 3wt%;
In the dispersible pigment color paste, the navy pigment content is 20wt%, and dispersant is 5wt%, and auxiliary agent is 0.1wt%, and balance solvent is DMAc, and granules of pigments is less than 1 μ m.
Adopt the preceding injected system of spinning of embodiment 1 or 2, regulate stoste and mill base measuring pump flow and guarantee that the pigment ratio is 3.0wt% in the fiber, above-mentioned painted stoste is carried out wet spinning, coagulation forming in 25 ℃ spinning bath, spinning bath consists of: 20wt%DMAc, 3wt% calcium chloride and 77wt% water, again by stretching, washing, oven dry, heat treatment, curl and cut-out, packing etc. become original liquid coloring navy meta-aramid finished fiber.
Embodiment 5
Injection technique was made original liquid coloring black meta-aramid fibers before employing was spun.
In the meta-aramid stoste, poly concentration is 18%, and dicyandiamide solution is DMAc/CaCl 2, CaCl wherein 2Concentration is 9wt%;
With with stoste in identical solvent stoste is diluted, being diluted to poly concentration is 6wt%, adds carbon black and disperse to make dispersible pigment color paste, the content of carbon black is the 20wt% of dispersible pigment color paste, granules of pigments is less than 1 μ m.
Adopt the preceding injected system of spinning of embodiment 1 or 2, regulate stoste and mill base measuring pump flow and guarantee that the pigment ratio is 4wt% in the fiber, above-mentioned painted stoste is carried out wet spinning.Coagulation forming in 110 ℃ spinning bath, spinning bath consists of: 15wt%DMAc, 40wt% calcium chloride and 45wt% water, again by modified, stretching, washing, oven dry, heat treatment, curl and cut-out, packing etc. become original liquid coloring black meta-aramid finished fiber.
Embodiment 6
Injection technique was made the yellow meta-aramid fibers of original liquid coloring before employing was spun.
In the meta-aramid stoste, poly concentration is 20wt%, and dicyandiamide solution is DMAc/CaCl 2, CaCl wherein 2Concentration is 3wt%;
With with stoste in identical solvent stoste is diluted, being diluted to poly concentration is 5wt%, adds granules of pigments and disperse to make dispersible pigment color paste, the content of granules of pigments is the 20wt% of dispersible pigment color paste, particle is less than 1 μ m.
Adopt the preceding injected system of spinning of embodiment 1 or 2, regulate stoste and mill base measuring pump flow and guarantee that the pigment weight ratio is 1.7wt% in the fiber, coagulation forming in 22 ℃ spinning bath, spinning bath consists of: 35wt%DMAc, 20wt% calcium chloride and 45wt% water, again by stretching, washing, oven dry, heat treatment, curl and cut-out, packing etc. become the yellow meta-aramid finished fiber of original liquid coloring.
Embodiment 7
Injection technique was made original liquid coloring black meta-aramid fibers before employing was spun.
In the meta-aramid stoste, poly concentration is 20wt%, and dicyandiamide solution is DMAc/CaCl 2, CaCl wherein 2Concentration is 3wt%;
With with stoste in identical solvent stoste is diluted, being diluted to poly concentration is 4wt%, adds carbon black and disperse to make dispersible pigment color paste, the content of carbon black is the 20wt% of dispersible pigment color paste, carbon black granules is less than 1 μ m.
Adopt the preceding injected system of spinning of embodiment 1 or 2, regulate stoste and mill base measuring pump flow and guarantee that the carbon black part by weight is 4.0wt% in the fiber, above-mentioned painted stoste is carried out dry spinning, again by washing, oven dry, heat treatment, curl and cut-out, packing etc. become original liquid coloring black meta-aramid finished fiber.
Embodiment 8
Injection technique was made original liquid coloring navy meta-aramid fibers before employing was spun.
In the meta-aramid stoste, poly concentration is 20wt%, and dicyandiamide solution is DMAc/CaCl 2, CaCl wherein 2Concentration is 9wt%;
In the dispersible pigment color paste, the navy pigment content is 20wt%, and dispersant is 5wt%, and auxiliary agent is 0.1wt%, and surplus is solvent DMAc, and granules of pigments is less than 1 μ m.
Adopt the preceding injected system of spinning of embodiment 1 or 2, regulate stoste and mill base measuring pump flow and guarantee that the pigment ratio is 3.0wt% in the fiber, above-mentioned painted stoste is carried out dry spinning, again by washing, oven dry, heat treatment, curl and cut-out, packing etc. become original liquid coloring navy meta-aramid finished fiber.

Claims (10)

1, injection technique was made the method for spun dyeing meta-aramid fiber before a kind of employing was spun, it is characterized in that: be provided with in position and spin preceding injected system near spinning machine, injected system comprised meta-aramid stoste measuring pump before this spun, the dispersible pigment color paste measuring pump, blender, pressurizer and pressure automatic control system, wherein, blender is an one-level blender, or two one-level blender and secondary blenders of connecting in regular turn, after on-line continuous ground will measure through the meta-aramid stoste of filtration and deaeration and dispersible pigment color paste, send into blender together and disperse and mix, mixed painted stoste is carried out spinning through being delivered to spinning machine behind the pressurizer.
2, injection technique was made the method for spun dyeing meta-aramid fiber before employing according to claim 1 was spun, and it is characterized in that: described measuring pump adopts a kind of in gear wheel metering pump, diaphragm metering pump, plunger metering pump, the screw pump.
3, injection technique was made the method for spun dyeing meta-aramid fiber before employing according to claim 1 was spun, it is characterized in that: described one-level blender is static mixer or rotor/stator high-shear mixer, and described secondary blender is static mixer or rotor/stator high-shear mixer.
4, injection technique was made the method for spun dyeing meta-aramid fiber before employing according to claim 1 was spun, it is characterized in that: described pressurizer comprises painted stoste import, the outlet of painted stoste, compressed air import and export, manometer, pressure transmitter and liquid level gauge, painted stoste import is connected with the outlet of blender, and outlet is connected with spinning machine.
5, injection technique was made the method for spun dyeing meta-aramid fiber before employing according to claim 4 was spun, it is characterized in that: described pressurizer is a sealed pressure vessel, wherein be sealed with compressed air, one closed loop robot control system(RCS) detected pressures balancer inner air pressure and painted stoste liquid level, and corresponding adjusting meta-aramid stoste and dispersible pigment color paste measuring pump flow, make that painted stoste pressure stability keeps the proportions constant of meta-aramid stoste and dispersible pigment color paste constant at certain level simultaneously in the pressurizer.
6, injection technique was made the method for spun dyeing meta-aramid fiber before employing according to claim 1 was spun, and it is characterized in that: described meta-aramid stoste is 1: 0.0002~0.5000 with the mixing quality ratio of dispersible pigment color paste.
7, injection technique was made the method for spun dyeing meta-aramid fiber before employing according to claim 6 was spun, it is characterized in that: in the described meta-aramid stoste, the mass concentration of poly is 5~25%, dicyandiamide solution is dimethylacetylamide or dimethylacetylamide/calcium chloride system, dimethylacetylamide/calcium chloride dicyandiamide solution comprises the low salt system of calcium chloride mass concentration≤3% and the high salt system of calcium chloride mass concentration>3%, and poly is by low temperature solution polymerization method or interfacial polymerization preparation.
8, injection technique was made the method for spun dyeing meta-aramid fiber before employing according to claim 6 was spun, it is characterized in that: described dispersible pigment color paste is the dispersion liquid of granules of pigments in solvent, solvent is dimethylacetylamide or dimethylacetylamide/calcium chloride, and dispersible pigment color paste comprises following component by weight percentage:
Pigment 5~25%
Dispersant 1~6%
Auxiliary agent 0.01~1.00%
Calcium chloride 0~9%
Dimethylacetylamide 59~93.99%,
Wherein, the granules of pigments particle diameter is less than 1 μ m, and pigment is one or more the combination in azo class, many lopps, the condensed ring class mineral-type pigment.
9, injection technique was made the method for spun dyeing meta-aramid fiber before employing according to claim 6 was spun, it is characterized in that: described dispersible pigment color paste is the dispersion liquid of granules of pigments in meta-aramid stoste dilution, dilution is identical with solvent in the stoste with solvent, and dispersible pigment color paste comprises following component by weight percentage:
Pigment 5~25%
Poly 0.1~25.0%
Calcium chloride 0.1~9.0%
Dimethylacetylamide 41~94.8%,
Wherein, the granules of pigments particle diameter is less than 1 μ m, and pigment is one or more the combination in azo class, many lopps, the condensed ring class mineral-type pigment.
10, injection technique was made the prepared painted meta-aramid fibers product of method of spun dyeing meta-aramid fiber before described employing was spun at one of claim 1 to 9, it is characterized in that: in the described painted meta-aramid fibers, the mass percent of pigment is 0.01~10.00%.
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CN106676644A (en) * 2015-11-05 2017-05-17 无锡索力得科技发展有限公司 Melt-direct spinning production system with addition of color sizing primary liquid
CN106676645A (en) * 2015-11-05 2017-05-17 无锡索力得科技发展有限公司 Production system of adding color paste stock solution by single box melt direct spinning
CN109416032A (en) * 2016-05-25 2019-03-01 嘉洛斯控股有限公司 Polymer material
CN110080014A (en) * 2019-04-12 2019-08-02 武汉纺织大学 A kind of method of meta-aramid particles of textiles stream dyeing
CN113005582A (en) * 2021-03-01 2021-06-22 华峰化学股份有限公司 Colorful spandex fiber and preparation method thereof
CN113005582B (en) * 2021-03-01 2022-08-16 华峰化学股份有限公司 Colorful spandex fiber and preparation method thereof

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