CN106637753A - Dyeing kettle and aramid fiber supercritical carbon dioxide waterless dyeing device and method - Google Patents

Dyeing kettle and aramid fiber supercritical carbon dioxide waterless dyeing device and method Download PDF

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Publication number
CN106637753A
CN106637753A CN201611039453.0A CN201611039453A CN106637753A CN 106637753 A CN106637753 A CN 106637753A CN 201611039453 A CN201611039453 A CN 201611039453A CN 106637753 A CN106637753 A CN 106637753A
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carbon dioxide
dyeing
dyestuff
carrier
aramid fiber
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CN106637753B (en
Inventor
郑来久
郑环达
高世会
闫俊
张娟
赵虹娟
熊小庆
吴劲松
李飞霞
韩益桐
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Taihe New Material Group Co ltd
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Dalian Polytechnic University
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06BTREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B1/00Applying liquids, gases or vapours onto textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing or impregnating
    • D06B1/02Applying liquids, gases or vapours onto textile materials to effect treatment, e.g. washing, dyeing, bleaching, sizing or impregnating by spraying or projecting
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06BTREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B23/00Component parts, details, or accessories of apparatus or machines, specially adapted for the treating of textile materials, not restricted to a particular kind of apparatus, provided for in groups D06B1/00 - D06B21/00
    • D06B23/14Containers, e.g. vats
    • D06B23/18Sealing arrangements
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06BTREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B23/00Component parts, details, or accessories of apparatus or machines, specially adapted for the treating of textile materials, not restricted to a particular kind of apparatus, provided for in groups D06B1/00 - D06B21/00
    • D06B23/20Arrangements of apparatus for treating processing-liquids, -gases or -vapours, e.g. purification, filtration, distillation

Abstract

The invention discloses a dyeing kettle and an aramid fiber supercritical carbon dioxide waterless dyeing device and method. A dyeing unit in the dyeing kettle includes a top sealing cover, a carbon dioxide fluid outlet pipe, an atomization sprayer I, an atomization channel, a porous center pipe, a bottom sealing cover, an atomization sprayer II and a carbon dioxide fluid inlet pipe. A blending device includes a carbon dioxide fluid inlet, a carrier or cosolvent inlet, a spinning impeller I, a blending grid I, a blending grid II, a honeycomb mixer, a rotary impeller II, and a carbon dioxide fluid outlet. According to the aramid fiber supercritical carbon dioxide waterless dyeing device, uniform mixing of a carrier or a cosolvent and a dye adjuvant can be achieved, the solubility of the dye adjuvant is thus increased, dyeing properties of aramid fibers are improved, and waterless and clean dyeing processing of the aramid fibers is finally achieved.

Description

A kind of dyeing caldron, aramid fiber supercritical carbon dioxide non-aqueous dyeing device and dyeing Method
Technical field
The present invention relates to carry out the anhydrous dye of aramid fiber using supercritical carbon dioxide fluid in a kind of textile dyeing and finishing industry The apparatus and method of color.
Background technology
The full name of aramid fiber is aromatic polyamide fibre.1974, U.S. trade federation (Federal Trade Commission) they are named as into " Aramid fibers ", its definition is:At least 85% acid amides chain (- CONH-) is straight Connect and be connected with two phenyl ring.Aramid fiber has excellent physicochemical characteristics as dual-use high-performance fiber new material, special It, with excellent heat-resisting quantity, anti-flammability, electrical insulating property, chemical resistance, radiation resistance and hot wet migration energy, is aviation not to be The important foundation material in the fields such as space flight, telecommunications, environmental protection, chemical industry and ocean development.
Dupont companies of the U.S. in 1956 start to spread out aramid fiber and study, nineteen sixty aramid fiber 1313 lab scale success, referred to as For HT-1, the pilot scale of input in 1963 formally starts industrialized production, trade name Nomex for 1967, and production scale is 450 tons/ Year, increase to 250,000,000 tons/year within 1993.Meanwhile, also complete the production of Fanglun l414 fiber, trade name " Kevlar ". Development of the Japanese TeiJin companies through more than ten years also successfully develops the essentially identical aramid fiber 1313 of structure, business in 1970 The name of an article is Conex, possesses 28450 tons/year of production capacity.China has started the development of aramid fiber, the Chinese Academy of Sciences, Tsing-Hua University in 1972 Successively aramid fiber PRODUCTION TRAITS is carried out Deng scientific research institutions.Wherein, 2000, Yantai Tayho Advanced Materials Co., Ltd. from Kazakhstan introduces correlation technique, software and starts to explore aramid fiber 1313 production;In March, 2003 has built 500 tons/year of tools There is the aramid fiber 1313 pilot production line of independent intellectual property right;And put into serial production in May, 2004, trade name " Niu Shida ", cut To current production capacity up to 7000 tons/year, become the leading enterprise of China's aramid fiber production, and in world's meta virtue It is at the second place in synthetic fibre supplier.
In recent years, the production technology of aramid fiber 1313 has more tended to ripe, and sustained production increases, and its range of application is also continuous Expand, such as high-temperature-resistant filtering material, electrical apparatus insulation material, honeycomb structure material and fire proofing material.Meanwhile, aramid fiber 1313 product The field of taking is increasingly being used to, such as space suit, fire-entry suit, racing car clothes, field operations take contour performance textile so that its dyeing Demand gradually increases.However, aramid fiber 1313 have high vitrification point (>250 DEG C) and the extremely difficult realization dye in aqueous medium Color, and serious discoloration is also easy to produce under illumination condition due to dyeing aramid fiber 1313, cause aramid fiber dyeing product Fastness to light is poor, and the problems referred to above significantly limit application of the aramid fiber 1313 in textile garment field.
The content of the invention
The present invention is directed to the problems referred to above, there is provided a kind of aramid fiber supercritical carbon dioxide non-aqueous dyeing device and side Method, to solve a dyeing difficult problem for aramid fiber, realizes that it cleans dyeing production.
The present invention provides a kind of dyeing caldron, and the dye unit in dyeing caldron is cylindrical shape, includes top successively from top to bottom Capping, nebulization channel, bottom cover, the nebulization channel is porous plate, and with top closure cylindrical space is formed, and the atomization is led to Road is connected porous central tube with bottom cover center;CO 2 fluid inlet tube enters poriferous circular through bottom cover Pipe, CO 2 fluid inlet tube is provided with atomizer II at close bottom cover;The top closure is provided with titanium dioxide Carbon fluid outlet pipe, the CO 2 fluid inlet tube is provided with atomizer I at close top closure;The carbon dioxide Connect finishing agent inlet tube on fluid inlet tube;Atomizer is provided with the finishing agent inlet tube.In achievable dyeing course The interior dye of supercritical carbon dioxide, dyestuff and carrier/cosolvent three-phase mixture, the two-way inflow of outer dye, it is fine so as to improve aramid fiber The dyeability of dimension.Wherein, atomizer I is divergence form, and atomizer II is vertical-type.
The present invention is provided with a kind of aramid fiber supercritical carbon dioxide non-aqueous dyeing device, including:Carbon dioxide remittance gas Row, CO2 heater, condenser, carbon dioxide storage tank, forecooler, carbon dioxide pressurization pump, carrier/cosolvent pump, load Dye described in body/cosolvent tank, co 2 heat exchanger, heat-conducting oil system, supplementary heat-conducting oil system, dyestuff kettle, claim 1 Kettle, magnetic force circulating pump, separator, glycol head tank, cooling tower, cold rinse bank, water pump, compressor and eg pump.
Further, in above-mentioned technical proposal, the aramid fiber supercritical carbon dioxide non-aqueous dyeing device, it is special Levy and be:Including blender, the blender be cylinder, front end include CO 2 fluid entrance, carrier/cosolvent entrance, It is internal to include rotary blade I, blending grid I, blending grid II, honeycomb blender, rotary blade II and carbon dioxide stream successively Body outlet;The blending grid I is the multipipe structure of both ends open, manages the cylinder non-horizontal or vertical with blender is;Institute State multipipe structure of the blending grid II for both ends open, the pipe direction of the blending grid II and the pipe direction phase of blending grid I It is right;The honeycomb blender is many sky honeycombs.Rotation blending grid I, blending grid II and the mixing of honeycomb blender three-level Unit, under the stirring action of rotary blade I and rotary blade II, realizes supercritical carbon dioxide, dyestuff and carrier/cosolvent The uniform mixing of three-phase mixture.
Further, in above-mentioned technical proposal, a kind of described aramid fiber supercritical carbon dioxide non-aqueous dyeing dress Put, it is characterised in that blending grid I, blending grid II and honeycomb blender aperture be respectively 0.01um, 0.01um and 0.001um。
The present invention provides a kind of method dyeed using above-mentioned aramid fiber supercritical carbon dioxide non-aqueous dyeing device, its It is characterised by:Carbon dioxide in gas cylinder flows through bus-bar in the presence of heater, and is cooled to liquid two through condenser Carbon oxide fluid is stored in carbon dioxide recycle tank, so that dyeing course is used;When textile dyeing is produced, in circulating tank Carbon dioxide first flows through forecooler condensation, and is entered inside dyeing installation by carbon dioxide pressurization infusion, completes boost process; Heat exchanger is recycled to heat CO 2 fluid so that it enters supercriticality;Supercritical carbon dioxide fluid is first The dyestuff or carrier/cosolvent dissolved in it is introduced in dyestuff kettle;And the liquid entered with carrier/cosolvent infusion in blender State carrier/cosolvent mixing;Supercritical carbon dioxide, dyestuff, carrier/cosolvent three-phase mixture flows into the dyeing in dyeing caldron Kevlar fabric is contaminated on unit, the CO 2 fluid containing dyestuff and carrier/cosolvent in the presence of circulating pump is in dyestuff kettle Circulate and between dyeing and finishing kettle, so as to complete dyeing course;After the completion of dyeing and finishing process, CO 2 fluid is by separating still and not The dyestuff depth of upper dye is separated;Again by condenser by pure carbon dioxide recovery to carbon dioxide storage tank.
Further, in above-mentioned technical proposal, the aramid fiber is selected from aramid fiber 1313, Fanglun l414 and PSA fiber.
Further, in above-mentioned technical proposal, aramid fiber is wrapped in the poriferous circular of the dye unit in dyeing caldron In the dyestuff cylinder that Guan Shang, dyestuff and solid-state carrier are placed in dyestuff kettle, liquid-carrier is placed in carrier/cosolvent tank.It is overcritical CO 2 fluid initially enters the dyestuff or solid carrier dissolved in dyestuff kettle in it;And in blender with carrier/altogether molten The liquid carrier that agent infusion enters/cosolvent mixing.
Further, in above-mentioned technical proposal, dyeing temperature is 100-200 DEG C, and dyeing pressure is 20-40MPa, is dyeed Time is 10-120min, and dye dosage is 1-5.5%, and CO 2 fluid flow is 10-1000g/min, carrier/cosolvent Flow is 1-50g/min.
Further, in above-mentioned technical proposal, the dyestuff is selected from disperse dyes, dispersible cationic dyestuff and cation Dyestuff.
Further, in above-mentioned technical proposal, the carrier/cosolvent is selected from dimethyl terephthalate (DMT), CINDYE DNK, ethanol and methyl alcohol.
Invention beneficial effect
(1) dye unit of invention is built-in with upper and lower two atomizers, and in dyeing course overcritical dioxy can be capable of achieving Change interior dye, the two-way inflow of outer dye of carbon, dyestuff and carrier/cosolvent three-phase mixture, and three-phase mixture can be ensured to fiber Uniform scattering and permeating, so as to improve the dyeability of aramid fiber.
(2) blender of invention includes blending grid I, blending grid II and honeycomb blender three-level mixed cell, can be with Under the stirring action of rotary blade I and rotary blade II, supercritical carbon dioxide, dyestuff and carrier/cosolvent three-phase is realized The uniform mixing of mixture;The addition of carrier, increased the solubility of dyestuff and reduces the vitrification point of aramid fiber, from And improve the dyeability of aramid fiber.
Description of the drawings
Fig. 1 is a kind of aramid fiber supercritical carbon dioxide non-aqueous dyeing schematic device;
Fig. 2 is the blender schematic diagram in a kind of anhydrous quick equipment for dyeing and finishing of supercritical carbon dioxide fluid;
Fig. 3 is that the dye unit in a kind of anhydrous quick equipment for dyeing and finishing of supercritical carbon dioxide fluid in dyeing caldron is illustrated Figure;
In figure, 1, carbon dioxide converge gas row;2nd, CO2 heater;3rd, condenser;4th, carbon dioxide storage tank;5th, precooling Device;6th, carbon dioxide pressurization pump;7th, co 2 heat exchanger;8th, heat-conducting oil system;9th, heat-conducting oil system is supplemented;10th, dyestuff kettle; 11st, carrier/cosolvent tank;12nd, carrier/cosolvent pump;13rd, blender;14th, dyeing caldron;15th, magnetic force circulating pump;16th, separate Device;17th, glycol head tank;18th, cooling tower;19th, cold rinse bank;20th, water pump;21st, compressor;22nd, eg pump;
131st, CO 2 fluid entrance;132nd, carrier/cosolvent entrance;133rd, rotary blade I;134th, grid I is blended; 135th, grid II is blended;136th, honeycomb blender;137th, rotary blade II;138th, CO 2 fluid outlet;
141st, top closure;142nd, CO 2 fluid outlet;143rd, atomizer I;144th, nebulization channel;145th, it is many Hole central tube;146th, atomizer II;147th, bottom cover and 148, CO 2 fluid inlet tube.
Specific embodiment
Below in conjunction with the specific embodiment of accompanying drawing 1, the accompanying drawing 2 and accompanying drawing 3 narration present invention in detail.
Embodiment 1
Carbon dioxide in gas cylinder flows through bus-bar in the presence of CO2 heater 2, and cold through condenser 3 But it is stored in carbon dioxide storage tank 4 for flow of liquid carbon dioxide body, so that dyeing and finishing process is used.When textile dyeing and finishing is produced, Carbon dioxide in carbon dioxide storage tank 4 first flows through forecooler 5 and condenses, and is set by the injection dyeing of carbon dioxide pressurization pump 6 It is standby internal, complete boost process;Co 2 heat exchanger 7 is recycled to heat CO 2 fluid so that it enters the excess of imports Critical condition;
Disperse red 60 is placed in the dyestuff cylinder of dyestuff kettle 10 with carrier dimethyl terephthalate (DMT), and its consumption is respectively fabric The 2% of weight and 3%.100kg aramid fiber 1313 fabrics are wrapped on the porous central tube 145 of dye unit.Before dyeing, beat first The bottom V15 valves of dyeing caldron 14 are opened, to empty the air in kettle and pipeline.During dyeing, supercritical carbon dioxide fluid enters Enter the dyestuff and carrier dissolved in dyestuff kettle 10 in it.Subsequently, supercritical carbon dioxide fluid is through V14 valves, by dyeing caldron bottom The CO 2 fluid inlet tube in portion enters dye unit, by atomizer II 146 by supercritical carbon dioxide, dyestuff and load Body three-phase mixture mixes dispersion and sprays into inside porous central tube 145, so as to the interior dye for carrying out aramid fiber 1313 fabric is dyeed.It is super to face Boundary's CO 2 fluid is flowed out by CO 2 fluid outlet, through V34, V17 and V19 valve, in magnetic force circulating pump 15 In the presence of flow back to dyestuff kettle 10, carry out 140 DEG C, the interior dye dye cycle of 30MPa, 30min.V34 valves are closed, it is overcritical CO 2 fluid is entered through V116 valves by the top of dyeing caldron 14, and is exported by the CO 2 fluid of dye unit Pipe 142 enters dye unit, and nebulization channel is entered with dispersed three-phase mixture by atomizer I 143, and by atomization The micropore of the bottom of passage 144 realizes outer dye dyeing course to aramid fiber 1313 fabric scattering and permeating.Supercritical carbon dioxide fluid by CO 2 fluid inlet tube 148 flows out, and through V14, V16, V17 and V19 valve, flows in the presence of magnetic force circulating pump 15 Dyestuff kettle 10 is returned, 140 DEG C, the dye cycle of 30MPa, 30min is carried out.
After dyeing terminates, dyestuff kettle 10 is closed, clean CO 2 fluid is passed through again, to elute aramid fiber 1313 fabric The dyestuff and carrier of attachment in surface and dyeing apparatus and pipeline.Dyeing caldron is kept in supercritical carbon dioxide fluid cleaning process Temperature 70 C, pressure 16MPa, scavenging period 20min.After the completion of aramid fiber 1313 fabric cleaning technique, overcritical titanium dioxide is reduced The temperature and pressure of carbon flow body, in 25 DEG C -40 DEG C of dyeing caldron temperature, under conditions of 3MPa-4MPa so that supercritical carbon dioxide Fluid and the dyestuff of dissolving, carrier are separated in the separator.Carbon dioxide returns carbon dioxide storage tank 4, in case under It is secondary to use.
After testing, dye aramid fiber 1313 textile dyeing depth and reach more than 5, dye level standard deviation is less than 0.1%.Its Washing color fastness, colour fastness to rubbing can reach more than 4 grades, and colour fasteness to sunlight reaches more than 6 grades.
Embodiment 2
Carbon dioxide in gas cylinder flows through bus-bar in the presence of CO2 heater 2, and cold through condenser 3 But it is stored in carbon dioxide storage tank 4 for flow of liquid carbon dioxide body, so that dyeing and finishing process is used.When textile dyeing and finishing is produced, Carbon dioxide in carbon dioxide storage tank 4 first flows through forecooler 5 and condenses, and is set by the injection dyeing of carbon dioxide pressurization pump 6 It is standby internal, complete boost process;Co 2 heat exchanger 7 is recycled to heat CO 2 fluid so that it enters the excess of imports Critical condition;
Dispersible cationic is bright blue to be placed in the dyestuff cylinder of dyestuff kettle 10, and its consumption is the 1% of fabric weight.Support C INDYE DNK is placed in carrier/cosolvent tank 11.500kg aramid fiber 1313s staple in bulk is put on the porous central tube 145 of dye unit In dyeing caldron.Before dyeing, the bottom V15 valves of dyeing caldron 14 are first turned on, to empty the air in kettle and pipeline.Dyeing When, supercritical carbon dioxide fluid enters in dyestuff kettle 10 dyestuff dissolved in it.Support C INDYE DNK is through carrier/altogether molten Agent pump 12 enters carrier/cosolvent entrance 132 with the flow velocity of 50g/min;The CO 2 fluid for being dissolved with dyestuff passes through dioxy Change carbon fluid intake 131 and enter blender 13;Carrier and supercritical carbon dioxide fluid are first in the effect of rotary blade I 133 Under tentatively mixed, then pass sequentially through blending grid I 134, blending grid II 135 and the three-level of honeycomb blender 136 mixing Unit is sufficiently mixed, and the solubility of dyestuff is improved in the presence of carrier.Subsequently, supercritical carbon dioxide fluid is passed through V14 valves, by the CO 2 fluid inlet tube 148 of the bottom of dyeing caldron 14 dye unit is entered, will be super by atomizer II 146 Critical carbon dioxide, dyestuff and carrier three-phase mixture mix dispersion and spray into inside porous central tube 145, so as to carry out aramid fiber The interior dye dyeing of 1313 staple in bulks.Supercritical carbon dioxide fluid is flowed out by CO 2 fluid outlet 142, through V34, V17 and V19 valves, flow back to dyestuff kettle 10 in the presence of magnetic force circulating pump 15, carry out 160 DEG C, the dyeing of 30MPa, 90min Circulation.
After dyeing terminates, dyestuff kettle 10 is closed, clean CO 2 fluid is passed through again, to elute aramid fiber 1313 fabric The dyestuff of attachment in surface and dyeing apparatus and pipeline.Dyeing caldron temperature 60 is kept in supercritical carbon dioxide fluid cleaning process DEG C, pressure 14MPa, scavenging period 20min.After the completion of aramid fiber 1313 staple in bulk cleaning, stream of supercritical carbon dioxide is reduced The temperature and pressure of body, in 25 DEG C -40 DEG C of dyeing caldron temperature, under conditions of 3MPa-4MPa so that supercritical carbon dioxide fluid Separated in separator 16 with the dyestuff of dissolving.Carbon dioxide returns carbon dioxide storage tank 4, in case using next time.
After testing, dye aramid fiber loose stock dyeing depth and reach more than 6, dye level standard deviation is less than 0.15%.Its Washing color fastness, colour fastness to rubbing can reach more than 4-5 levels;Colour fasteness to sunlight can reach more than 6 grades.
Embodiment 3
Carbon dioxide in gas cylinder flows through bus-bar in the presence of CO2 heater 2, and cold through condenser 3 But it is stored in carbon dioxide storage tank 4 for flow of liquid carbon dioxide body, so that dyeing and finishing process is used.When textile dyeing and finishing is produced, Carbon dioxide in carbon dioxide storage tank 4 first flows through forecooler 5 and condenses, and is set by the injection dyeing of carbon dioxide pressurization pump 6 It is standby internal, complete boost process;Co 2 heat exchanger 7 is recycled to heat CO 2 fluid so that it enters the excess of imports Critical condition;
Cationic Yellow X-6G is placed in the dyestuff cylinder of dyestuff kettle, and its consumption is 1%.Support C INDYE DNK be placed in carrier/ In cosolvent tank.400kg Fanglun l414s staple in bulk is placed in dyeing caldron around the porous central tube of dye unit.It is first before dyeing Dyeing caldron bottom V15 valves are first opened, to empty the air in kettle and pipeline.During dyeing, supercritical carbon dioxide fluid The dyestuff in it is dissolved in dyestuff kettle.Support C INDYE DNK through cosolvent pump with the flow velocity of 10g/min enter carrier/ Cosolvent entrance;The CO 2 fluid for being dissolved with dyestuff enters blender by CO 2 fluid entrance;Carrier faces with super Boundary's CO 2 fluid is tentatively mixed first in the presence of rotary blade I, then passes sequentially through blending grid I, blending Grid II and honeycomb blender three-level mixed cell are sufficiently mixed, and the solubility of dyestuff is improved in the presence of carrier.With Afterwards, supercritical carbon dioxide fluid enters dye unit through V14 valves by the CO 2 fluid inlet tube of dyeing caldron bottom, Supercritical carbon dioxide, dyestuff and carrier three-phase mixture are mixed into dispersion by atomizer II to spray in porous central tube Portion, so as to the interior dye for carrying out Fanglun l414 staple in bulk is dyeed.Supercritical carbon dioxide fluid is by CO 2 fluid outlet stream Go out, through V34, V17 and V19 valve, dyestuff kettle flowed back in the presence of magnetic force circulating pump, carry out 160 DEG C, 30MPa, The dye cycle of 90min.
After dyeing terminates, dyestuff kettle is closed, clean CO 2 fluid is passed through again, to elute Fanglun l414 staple in bulk The dyestuff and carrier of attachment in surface and dyeing apparatus and pipeline.Dyeing caldron is kept in supercritical carbon dioxide fluid cleaning process Temperature 60 C, pressure 14MPa, scavenging period 20min.After the completion of Fanglun l414 staple in bulk cleaning, overcritical dioxy is reduced Change the temperature and pressure of carbon flow body, in 25 DEG C -40 DEG C of dyeing caldron temperature, under conditions of 3MPa-4MPa so that overcritical titanium dioxide Carbon flow body and the dyestuff of dissolving are separated in the separator.Carbon dioxide returns carbon dioxide storage tank, in case making next time With.
After testing, dye Fanglun l414 loose stock dyeing depth and reach more than 3.5, dye level standard deviation is less than 0.12, with preferable level-dyeing property feature.Meanwhile, coloured fibre washing color fastness, colour fastness to rubbing can reach 4-5 levels with On, colour fasteness to sunlight can reach more than 6 grades.
Embodiment 4
Carbon dioxide in gas cylinder flows through bus-bar in the presence of CO2 heater 2, and cold through condenser 3 But it is stored in carbon dioxide storage tank 4 for flow of liquid carbon dioxide body, so that dyeing and finishing process is used.When textile dyeing and finishing is produced, Carbon dioxide in carbon dioxide storage tank 4 first flows through forecooler 5 and condenses, and is set by the injection dyeing of carbon dioxide pressurization pump 6 It is standby internal, complete boost process;Co 2 heat exchanger 7 is recycled to heat CO 2 fluid so that it enters the excess of imports Critical condition;
Disperse Blue-56 is placed in the dyestuff cylinder of dyestuff kettle, and its consumption is respectively 3%.Carrier ethyl alcohol is placed in carrier/cosolvent In tank.500kg PSA fiber cheeses are enclosed within the porous central tube of dye unit.Before dyeing, dyeing caldron bottom V15 is first turned on Number valve, to empty the air in kettle and pipeline.During dyeing, supercritical carbon dioxide fluid is entered in dyestuff kettle and dissolved in it Dyestuff.Carrier enters through cosolvent pump and enters blender with the flow velocity of 30g/min.It is dissolved with the titanium dioxide of dyestuff and carrier Carbon flow body enters blender by CO 2 fluid entrance, is tentatively mixed in the presence of rotary blade I first, then Pass sequentially through blending grid I, blending grid II and honeycomb blender three-level mixed cell to be sufficiently mixed, in the effect of carrier The lower solubility for improving dyestuff.Subsequently, supercritical carbon dioxide fluid is entered through V116 valves by dyeing caldron top, and Dye unit is entered by the CO 2 fluid outlet of dye unit, enters nebulization channel uniformly to divide by atomizer I Scattered three-phase mixture, and by the micropore of nebulization channel bottom to PSA fiber cheese scattering and permeating, realize outer dye dyeing course. Supercritical carbon dioxide fluid is flowed out by CO 2 fluid inlet tube, through V14, V16, V17 and V19 valve, in magnetic force Dyestuff kettle is flowed back in the presence of circulating pump, 140 DEG C, the dye cycle of 35MPa, 60min is carried out.
After dyeing terminates, dyestuff kettle is closed, clean CO 2 fluid is passed through again, to elute aramid fiber 1313 cheese The dyestuff and carrier of attachment in surface and dyeing apparatus and pipeline.Dyeing caldron is kept in supercritical carbon dioxide fluid cleaning process 80 DEG C of temperature, pressure 16MPa, scavenging period 10min.After the completion of PSA fiber cheese cleaning, overcritical titanium dioxide is reduced The temperature and pressure of carbon flow body, in 25 DEG C -40 DEG C of dyeing caldron temperature, under conditions of 3MPa-4MPa so that supercritical carbon dioxide Fluid and the dyestuff of dissolving are separated in the separator.Carbon dioxide returns carbon dioxide storage tank, in case using next time.
After testing, dye PSA fiber cheese dyeing depth and reach more than 4, dye level standard deviation is less than 0.16, tool There is preferable level-dyeing property feature.Meanwhile, coloured fibre washing color fastness, colour fastness to rubbing can reach more than 4 grades, sun-resistant Color fastness can reach more than 6 grades.
Embodiment 5
Carbon dioxide in gas cylinder flows through bus-bar in the presence of CO2 heater 2, and cold through condenser 3 But it is stored in carbon dioxide storage tank 4 for flow of liquid carbon dioxide body, so that dyeing and finishing process is used.When textile dyeing and finishing is produced, Carbon dioxide in carbon dioxide storage tank 4 first flows through forecooler 5 and condenses, and is set by the injection dyeing of carbon dioxide pressurization pump 6 It is standby internal, complete boost process;Co 2 heat exchanger 7 is recycled to heat CO 2 fluid so that it enters the excess of imports Critical condition;
DISPERSE Yellow 211 is placed in the dyestuff cylinder of dyestuff kettle, and its consumption is 4%.Carrier methyl alcohol is placed in carrier/cosolvent tank It is interior.Aramid fiber 1313 fabric is wrapped on the porous central tube of dye unit.Before dyeing, dyeing caldron bottom V15 valves are first turned on Door, to empty the air in kettle and pipeline.During dyeing, supercritical carbon dioxide fluid enters in dyestuff kettle the dye dissolved in it Material.Carrier enters through cosolvent pump and enters blender with the flow velocity of 40g/min.It is dissolved with the carbon dioxide stream of dyestuff and carrier Body enters blender by CO 2 fluid entrance, is tentatively mixed in the presence of rotary blade I first, then successively It is sufficiently mixed by the way that grid I, blending grid II and honeycomb blender three-level mixed cell is blended, is carried in the presence of carrier The solubility of high dyestuff.Subsequently, supercritical carbon dioxide fluid is entered through V116 valves by dyeing caldron top, and by contaminating The CO 2 fluid outlet of color element enters dye unit, and nebulization channel is entered with dispersed three by atomizer I Body is mixed, and by the micropore of nebulization channel bottom to aramid fiber 1313 fabric scattering and permeating, realizes outer dye dyeing course.It is super to face Boundary's CO 2 fluid is flowed out by CO 2 fluid inlet tube, through V14, V16, V17 and V19 valve, in magnetic force circulation Dyestuff kettle is flowed back in the presence of pump, 180 DEG C, the dye cycle of 40MPa, 70min is carried out.
After dyeing terminates, dyestuff kettle is closed, clean CO 2 fluid is passed through again, to elute aramid fiber 1313 fabric table The dyestuff and carrier of attachment in face and dyeing apparatus and pipeline.Dyeing kettle temperature is kept in supercritical carbon dioxide fluid cleaning process 60 DEG C of degree, pressure 15MPa, scavenging period 20min.After the completion of aramid fiber 1313 fabric cleaning technique, supercritical carbon dioxide is reduced The temperature and pressure of fluid, in 25 DEG C -40 DEG C of dyeing caldron temperature, under conditions of 3MPa-4MPa so that stream of supercritical carbon dioxide Body and the dyestuff of dissolving are separated in the separator.Carbon dioxide returns carbon dioxide storage tank, in case using next time.
After testing, dye aramid fiber 1313 textile dyeing depth and reach more than 6, dye level standard deviation is less than 0.1, has Preferable level-dyeing property feature.Meanwhile, coloured fibre washing color fastness, colour fastness to rubbing can reach more than 4-5 levels, sun-resistant Color fastness can reach more than 6 grades.
Embodiment 6
Carbon dioxide in gas cylinder flows through bus-bar in the presence of CO2 heater 2, and cold through condenser 3 But it is stored in carbon dioxide storage tank 4 for flow of liquid carbon dioxide body, so that dyeing and finishing process is used.When textile dyeing and finishing is produced, Carbon dioxide in carbon dioxide storage tank 4 first flows through forecooler 5 and condenses, and is set by the injection dyeing of carbon dioxide pressurization pump 6 It is standby internal, complete boost process;Co 2 heat exchanger 7 is recycled to heat CO 2 fluid so that it enters the excess of imports Critical condition;
Disperse Blue-79 and disperse red 60 with etc. mass ratio be placed in the dyestuff cylinder of dyestuff kettle, its consumption is 1%.Carrier N, N- Diethyl-m-methyl benzamide is placed in carrier/cosolvent tank.500kg Fanglun l414s staple in bulk is more around dye unit Hole central tube is placed in dyeing caldron.Before dyeing, dyeing caldron bottom V15 valves are first turned on, to empty in kettle and pipeline Air.During dyeing, supercritical carbon dioxide fluid enters in dyestuff kettle the dyestuff dissolved in it.Carrier N, a N- diethyl-first Yl-benzamide enters carrier/cosolvent entrance through cosolvent pump with the flow velocity of 20g/min;It is dissolved with the carbon dioxide of dyestuff Fluid enters blender by CO 2 fluid entrance;Carrier and supercritical carbon dioxide fluid are first in rotary blade I Tentatively mixed under effect, then pass sequentially through blending grid I, blending grid II and honeycomb blender three-level mixed cell and enter Row is sufficiently mixed, and the solubility of dyestuff is improved in the presence of carrier.Subsequently, supercritical carbon dioxide fluid is through V14 valves, by The CO 2 fluid inlet tube of dyeing caldron bottom enters dye unit, by atomizer II by supercritical carbon dioxide, dye Material and carrier three-phase mixture mix dispersion and spray into inside porous central tube, so as to the interior dye for carrying out Fanglun l414 staple in bulk contaminates Color.Supercritical carbon dioxide fluid is flowed out by CO 2 fluid outlet, through V34, V17 and V19 valve, is followed in magnetic force Dyestuff kettle is flowed back in the presence of ring pump, 170 DEG C, the dye cycle of 34MPa, 90min is carried out.
After dyeing terminates, dyestuff kettle is closed, clean CO 2 fluid is passed through again, to elute Fanglun l414 staple in bulk The dyestuff and carrier of attachment in surface and dyeing apparatus and pipeline.Dyeing caldron is kept in supercritical carbon dioxide fluid cleaning process Temperature 60 C, pressure 14MPa, scavenging period 20min.After the completion of Fanglun l414 staple in bulk cleaning, overcritical dioxy is reduced Change the temperature and pressure of carbon flow body, in 25 DEG C -40 DEG C of dyeing caldron temperature, under conditions of 3MPa-4MPa so that overcritical titanium dioxide Carbon flow body and the dyestuff of dissolving are separated in the separator.Carbon dioxide returns carbon dioxide storage tank, in case making next time With.
After testing, dye Fanglun l414 loose stock dyeing depth and reach more than 5, dye level standard deviation is less than 0.2, tool There is preferable level-dyeing property feature.Meanwhile, coloured fibre washing color fastness, colour fastness to rubbing can reach more than 4-5 levels, resistance to day Shine color fastness and can reach more than 6 grades.

Claims (10)

1. a kind of dyeing caldron, it is characterised in that:Dye unit in dyeing caldron is cylindrical shape, from top to bottom successively including top envelope Lid, nebulization channel, bottom cover, the nebulization channel is porous plate, and with top closure cylindrical space, the nebulization channel are formed It is connected porous central tube with bottom cover center;CO 2 fluid inlet tube enters porous central tube through bottom cover, CO 2 fluid inlet tube is provided with atomizer II at close bottom cover;The top closure is provided with carbon dioxide stream Body outlet, the CO 2 fluid inlet tube is provided with atomizer I at close top closure;The CO 2 fluid Connect finishing agent inlet tube on inlet tube;Atomizer is provided with the finishing agent inlet tube.
2. a kind of aramid fiber supercritical carbon dioxide non-aqueous dyeing device, including:Carbon dioxide remittance gas row, carbon dioxide heating Device, condenser, carbon dioxide storage tank, forecooler, carbon dioxide pressurization pump, carrier/cosolvent pump, carrier/cosolvent tank, dioxy Change carbon heat exchanger, heat-conducting oil system, supplement heat-conducting oil system, dyestuff kettle, dyeing caldron described in claim 1, magnetic force circulating pump, point From device, glycol head tank, cooling tower, cold rinse bank, water pump, compressor and eg pump.
3. aramid fiber supercritical carbon dioxide non-aqueous dyeing device according to claim 2, it is characterised in that:Including blending Device, the blender is cylinder, and front end includes that CO 2 fluid entrance, carrier/cosolvent entrance, inside include successively rotation Impeller I, blending grid I, blending grid II, honeycomb blender, rotary blade II and CO 2 fluid outlet;The blending Grid I is the multipipe structure of both ends open, manages the cylinder non-horizontal or vertical with blender is;The blending grid II is two ends The multipipe structure of opening, the pipe direction of the blending grid II is relative with the pipe direction of blending grid I;The honeycomb blender is Many sky honeycombs.
4. a kind of aramid fiber supercritical carbon dioxide non-aqueous dyeing device according to claim 3, it is characterised in that altogether The aperture of mixed grid I, blending grid II and honeycomb blender is respectively 0.01um, 0.01um and 0.001um.
5. using the method for aramid fiber supercritical carbon dioxide non-aqueous dyeing device dyeing described in Claims 2 or 3, its feature It is:Carbon dioxide in gas cylinder flows through bus-bar in the presence of heater, and is cooled to liquid titanium dioxide through condenser Carbon flow body is stored in carbon dioxide recycle tank, so that dyeing course is used;When textile dyeing is produced, the dioxy in circulating tank Change carbon and first flow through forecooler condensation, and entered inside dyeing installation by carbon dioxide pressurization infusion, complete boost process;It is sharp again CO 2 fluid is heated with heat exchanger so that it enters supercriticality;Supercritical carbon dioxide fluid enters first Enter the dyestuff or carrier/cosolvent dissolved in dyestuff kettle in it;And the liquid entered with carrier/cosolvent infusion in blender is carried Body/cosolvent mixing;Supercritical carbon dioxide, dyestuff, carrier/cosolvent three-phase mixture flows into the dye unit in dyeing caldron Upper dye kevlar fabric, the CO 2 fluid containing dyestuff and carrier/cosolvent in the presence of circulating pump is in dyestuff kettle and dye Circulate between whole kettle, so as to complete dyeing course;After the completion of dyeing and finishing process, CO 2 fluid is by separating still and not upper dye Dyestuff depth separate;Again by condenser by pure carbon dioxide recovery to carbon dioxide storage tank.
6. a kind of aramid fiber supercritical carbon dioxide non-aqueous dyeing method according to claim 5, it is characterised in that:Institute Aramid fiber is stated selected from aramid fiber 1313, Fanglun l414 and PSA fiber.
7. a kind of aramid fiber supercritical carbon dioxide non-aqueous dyeing method according to claim 5, it is characterised in that virtue On the porous central tube of the dye unit that synthetic fibre fiber is placed in dyeing caldron, the dyestuff cylinder that dyestuff and solid-state carrier are placed in dyestuff kettle Interior, liquid-carrier is placed in carrier/cosolvent tank.
8. a kind of aramid fiber supercritical carbon dioxide non-aqueous dyeing method according to claim 5, it is characterised in that dye Color temperature is 100-200 DEG C, and dyeing pressure is 20-40MPa, and dyeing time is 10-120min, and dye dosage is 1-5.5%, two Carbon oxide fluid flow is 10-1000g/min, and carrier/cosolvent flow is 1-50g/min.
9. a kind of aramid fiber supercritical carbon dioxide non-aqueous dyeing method according to claim 5, it is characterised in that:Institute Dyestuff is stated selected from disperse dyes, dispersible cationic dyestuff and the dye of positive ion.
10. a kind of aramid fiber supercritical carbon dioxide non-aqueous dyeing method according to claim 5, it is characterised in that: Carrier/the cosolvent is selected from dimethyl terephthalate (DMT), CINDYE DNK, ethanol and methyl alcohol.
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