CN111676628A - Supercritical carbon dioxide anhydrous dyeing system and dyeing method - Google Patents
Supercritical carbon dioxide anhydrous dyeing system and dyeing method Download PDFInfo
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- CN111676628A CN111676628A CN202010523492.8A CN202010523492A CN111676628A CN 111676628 A CN111676628 A CN 111676628A CN 202010523492 A CN202010523492 A CN 202010523492A CN 111676628 A CN111676628 A CN 111676628A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B9/00—Solvent-treatment of textile materials
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- D—TEXTILES; PAPER
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- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B23/00—Component 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
- D06B23/20—Arrangements of apparatus for treating processing-liquids, -gases or -vapours, e.g. purification, filtration, distillation
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B23/00—Component 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
- D06B23/20—Arrangements of apparatus for treating processing-liquids, -gases or -vapours, e.g. purification, filtration, distillation
- D06B23/22—Arrangements of apparatus for treating processing-liquids, -gases or -vapours, e.g. purification, filtration, distillation for heating
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- D—TEXTILES; PAPER
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- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B9/00—Solvent-treatment of textile materials
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B9/00—Solvent-treatment of textile materials
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Abstract
The invention provides a supercritical carbon dioxide anhydrous dyeing system and a dyeing method, which are characterized in that: the dyeing system comprises a dyeing module and a public module, wherein the dyeing module comprises a dyeing unit and a filtering unit, the dyeing unit comprises a dye kettle, a dyeing kettle, a circulating pump and a connecting pipeline, and the filtering unit comprises a cooler, a filter and a heat exchanger; the public module comprises a carbon dioxide storage and conveying unit, a refrigerating unit, a separation and recovery unit and a control unit; the dyeing module is connected with the public module through a connecting pipeline, and the other dyeing modules are sequentially connected in parallel. The dyeing method comprises the following steps of: deoiling, dyeing/oligomer removing, cooling, filtering, heating and color floating removing and separating. The low polymer can be removed in the dyeing process, the yield is improved, the generation of loose color is reduced, and the washing fastness and the rubbing fastness of the finished product can reach the requirements of the national relevant standards.
Description
Technical Field
The invention belongs to the technical field of dyeing equipment and dyeing processes, and particularly relates to a supercritical carbon dioxide anhydrous dyeing system and a supercritical carbon dioxide anhydrous dyeing method.
Background
In recent years, the supercritical carbon dioxide anhydrous dyeing technology is gradually replacing the traditional dyeing method, has the advantages of high efficiency, no pollution, high dye utilization rate and the like, and is the development direction of the future dyeing technology.
Chemical fibers inevitably produce oligomers during the production process, and the existence of the oligomers has a great influence on the quality of the supercritical carbon dioxide anhydrous dyeing. The terylene oligomer is mainly ethylene terephthalate cyclic trimer which is generally 1 to 3 percent of the fiber mass.
Through the dissolution and dispersion simulation experiment of the cyclic trimer in the supercritical carbon dioxide fluid, the following conclusion is reached: the solubility of trimer molecules in supercritical carbon dioxide fluid is low, and if the cyclic trimer can be completely dissolved in the supercritical carbon dioxide fluid, the highest concentration can reach more than 2 g/L; ② under the condition of 130 ℃/24MPa, the concentration is required to be reduced to 0.125 g/L to ensure that the cyclic trimer exists in a monomolecular state in most of time; ③ under the condition of 130 ℃/30MPa, the concentration is required to be reduced to 0.25 g/L to ensure that the cyclic tripolymer exists in a monomolecular state in most of time; and fourthly, the solubility of the cyclic trimer in the supercritical carbon dioxide fluid can be increased by increasing the pressure.
The traditional dyeing method comprises the following steps: dyeing-separation, because the oligomer can not be removed, the problem of oligomer pollution exists, and the oligomer is attached to the inner wall of equipment to cause the friction damage of a dyed object; the oligomer is attached to the surface of the dyed object, so that the yield is low; the oligomer is attached to the yarn, so that subsequent processing equipment is abraded, the woven fabric is poor in hand feeling, the uneven attachment of the oligomer causes uneven friction force and color difference, and white spots and cross tracks are easy to appear on the woven fabric.
In the traditional process, separation and recovery are directly carried out after dyeing is finished, and in the separation process, along with the reduction of pressure and temperature, residual dye dissolved in carbon dioxide fluid is coagulated after dyeing is balanced and adheres to the surface of a dyed object to cause color spots, so that the yield is influenced; the existence of flooding causes that the color washing fastness and the rubbing fastness can only reach 3.5 grades, and can not reach the requirement of the finished product fastness grade 4.
The traditional process has no deoiling procedure before dyeing, and the dyeing quality is influenced by dissolving an oiling agent in carbon dioxide, particularly the problem of outer layer color difference of the cheese is caused.
How to design a supercritical carbon dioxide anhydrous dyeing system and a dyeing method, which solve the problems in the prior art, is a technical problem faced by the invention.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a supercritical carbon dioxide anhydrous dyeing system and a supercritical carbon dioxide anhydrous dyeing method, oligomers can be removed in the dyeing process, the yield is improved, the generation of loose color is reduced, and the color washing fastness and the rubbing fastness of the dyed finished product meet the requirements of national relevant standards.
The purpose of the invention is realized by the following technical scheme:
the supercritical carbon dioxide anhydrous dyeing system is characterized by comprising a dyeing module and a public module, wherein the dyeing module comprises a dyeing unit and a filtering unit, the dyeing unit comprises a dye kettle, a dyeing kettle, a circulating pump and a connecting pipeline, and the filtering unit comprises a cooler, a filter and a heat exchanger; the public module comprises a carbon dioxide storage and conveying unit, a refrigerating unit, a separation and recovery unit and a control unit, wherein the carbon dioxide storage and conveying unit comprises a CO2 circulating storage tank and a low-temperature booster pump; the refrigerating unit comprises a refrigerant tank, a refrigerating compressor, a refrigerant pump, a cold water pump, a water cooling tower and a condenser; the dyeing module is characterized in that at least one dyeing module is arranged on one common module, one dyeing module is connected with the common module through a connecting pipeline, and the rest dyeing modules are sequentially connected in parallel.
The improvement of the technical scheme is as follows: the separation and recovery unit comprises a primary separation device and a secondary separation device, a connecting pipeline led out from the outlet end of the dye kettle is sequentially connected in series with the dye kettle, a cooler, a filter, a heat exchanger and a circulating pump and then connected to the inlet end of the dye kettle to form a small circulation, the cooler is cooled by external cooling water, and the heat exchanger is heated by heat-conducting oil; another path of connecting pipeline led out from the outlet end of the dyeing kettle is connected with the primary separation device, the secondary separation device, the condenser and the CO2The circulating storage tank and the low-temperature booster pump are sequentially connected in series and then connected to the inlet end of the dye kettle to form a large circulation; the condenser in the public module is connected with the refrigeration compressor, the refrigeration compressor leads out two loops, one loop is formed by connecting the refrigeration compressor in series with a water cooling tower and a cold water pump, and the other loop is formed by connecting the refrigeration compressor in series with a refrigerant tank and a refrigerant pump.
The technical scheme is further improved as follows: two connecting pipelines are led out from the outlet end of the circulating pump, wherein a valve I is arranged on the connecting pipeline connected to the inlet end of the dyeing kettle, a valve II is arranged on the connecting pipeline connected to the inlet end of the dyeing kettle, a valve III is arranged on the connecting pipeline from the outlet end of the dyeing kettle to the inlet end of the condenser, and a valve IV is arranged on the connecting pipeline from the outlet end of the dyeing kettle to the inlet end of the primary separating device.
The technical scheme is further improved as follows: has a CO2The outlet end of the storage tank is connected with the inlet end of a delivery pump, and the outlet end of the delivery pump is connected with the CO2The circulating storage tank is connected.
The technical scheme is further improved as follows: the control unit comprises a temperature sensor, a pressure gauge, a flowmeter, a liquid level meter, an electrical system and a PLC control system; the public module also comprises a safety alarm detection unit, and the safety alarm detection unit consists of an oxygen sensor and a multi-channel controller.
The technical scheme is further improved as follows: the dyeing kettle comprises a loose fiber dyeing storage frame, a cheese dyeing creel and a grey cloth dyeing support; the loose fiber dyeing storage frame and the cheese dyeing creel are of vertical structures, the grey cloth dyeing support is of a horizontal structure, a fluid inlet of the grey cloth dyeing support adopts a labyrinth mechanical sealing device and a quick opening part, a small magnetic motor driving shaft arranged on the quick opening part is connected with a magnetic block, and the tail end of the grey cloth dyeing support is provided with a magnetic driving block and is connected with the magnetic block on the small magnetic motor driving shaft.
The technical scheme is further improved as follows: the dye kettle comprises a dye kettle tank body and a dye bin therein, the dye bin comprises a shell, a top cover and a chassis, an airflow inlet is arranged on the chassis, the dye bin comprises a bottom cylindrical section, a bottom conical section and a cylindrical dye bin main body section which are sequentially connected from bottom to top, a flow equalizing function area, an oligomer separation function area, a dye storage function area and a molten dye temporary storage function area are arranged in the dye bin layer by layer from bottom to top, magnetic force ring sealing is adopted among the function areas, and a bottom baffle plate among the function areas is a microporous filter plate; the flow equalizing functional area comprises a flow equalizing plate arranged in the bottom end conical section, a plurality of flow dividing holes are uniformly distributed on the flow equalizing plate, and the oligomer separation functional area is a microporous material layer which is used for adsorbing oligomers and has a rough surface; the dye storage functional area comprises a grid bin arranged above the microporous material layer, and the grid bin is an integral structure made of a metal porous filtering material through sintering; the molten dye temporary storage functional area comprises filament clusters which are uniformly and densely distributed on the dye storage functional area.
The dyeing method using the supercritical carbon dioxide anhydrous dyeing system is characterized by comprising the following steps of:
deoiling, dyeing/oligomer removing, cooling, filtering, heating and color floating removing, and separating and recycling.
The improvement of the technical scheme is as follows: the deoiling procedure comprises the following steps: removing oil agent on the dyed object by using the extraction function of supercritical carbon dioxide; the dyed materials comprise chemical fibers, chemical fiber cheese and chemical fiber fabrics;
the dyeing oligomer removing procedure comprises the following steps: an adsorption filtering device is arranged at a carbon dioxide fluid outlet of the dyeing kettle, and oligomer monomers dissolved in the carbon dioxide fluid are forced to pass through the adsorption filtering device along with the dyeing process, so that the oligomer is separated out through adsorption and collision;
the temperature reduction, filtration and temperature rise floating color removal process comprises the following steps: the dyeing process temperature is 120-;
the separation and recovery step: when the dye in the carbon dioxide fluid is completely separated, the carbon dioxide fluid is separated and recovered.
Compared with the prior art, the invention has the following advantages and positive effects:
1. the invention relates to a supercritical carbon dioxide anhydrous dyeing system, which is characterized in that one set of dyeing modules are connected with a public module through a connecting pipeline, and the other dyeing modules can be connected in parallel in sequence according to needs. Therefore, the production capacity can be improved by only increasing the number of the configured dyeing modules by investing the public modules at one time, and the equipment investment is less.
2. The dyeing method of the invention is added with a deoiling procedure to remove the influence of the oil agent on the dyeing quality; adding an oligomer removing function in the dyeing process, and filtering out oligomers in an oligomer removing function area in a dyeing bin; and (4) adding a floating color removing procedure, and filtering out the dissolved dye in the carbon dioxide by cooling, filtering and heating for several times after dyeing is finished. The color fastness to washing and rubbing of the dyed finished product meet the requirements of the national relevant standards.
Drawings
FIG. 1 is a schematic view of a connection structure of a supercritical carbon dioxide anhydrous dyeing system according to the present invention;
FIG. 2 is a schematic diagram of a dye bin structure of a dye kettle in the supercritical carbon dioxide anhydrous dyeing system.
Detailed Description
Referring to fig. 1, the embodiment of the supercritical carbon dioxide anhydrous dyeing system comprises a dyeing module B and a public module A, wherein the dyeing module B comprises a dyeing unit and a filtering unit, the dyeing unit comprises a dye kettle, a dyeing kettle, a circulating pump and a connecting pipeline, and the filtering unit comprises a cooler, a filter and a heat exchanger. The public module A comprises a carbon dioxide storage and conveying unit, a refrigerating unit, a separation and recovery unit and a control unit, wherein the carbon dioxide storage and conveying unit comprises a CO2 circulating storage tank and a low-temperature booster pump. The refrigerating unit comprises a refrigerant tank, a refrigerating compressor, a refrigerant pump, a cold water pump, a water cooling tower and a condenser. In the embodiment shown in fig. 1, one set of the common module a is provided with two sets of dyeing modules B (one set of the common module a may also be provided with one or more sets of dyeing modules B as required), one set of the dyeing modules B is connected with the common module a through a connecting pipeline, and the other dyeing modules B are connected in parallel in sequence.
Specifically, the method comprises the following steps: the separation and recovery unit comprises a primary separation device and a secondary separation device, wherein the primary separation device is used for spiral gas-liquid gas-solid separation to complete oil-gas separation and gas-solid separation of large dye particles; the second-stage separation is adsorption/filtration separation, the bottom layer is an oil absorption felt, and the upper layer is a molecular sieve which is used as a final guarantee device for separating and recovering carbon dioxide.
A connecting pipeline is led out from the outlet end of the dye kettle, and is sequentially connected with the dyeing kettle, the cooler, the filter, the heat exchanger and the circulating pump in series and then connected to the inlet end of the dye kettle to form small circulation, the cooler is cooled by external cooling water, and the heat exchanger is heated by heat-conducting oil. Another path of connecting pipeline led out from the outlet end of the dyeing kettle is connected with the primary separation device, the secondary separation device, the condenser and the CO2The circulating storage tank and the low-temperature booster pump are sequentially connected in series and then connected to the inlet end of the dye kettle to form a large circulation. The condenser in the public module A is connected with the refrigeration compressor, the refrigeration compressor leads out two loops, one loop is connected with the water cooling tower and the cold water pump in series to form a loop, and the other loop is connected with the refrigerant tank and the refrigerant pump in series to form a loop.
Two connecting pipelines are led out from the outlet end of the circulating pump, wherein a valve I is arranged on the connecting pipeline connected to the inlet end of the dyeing kettle, a valve II is arranged on the connecting pipeline connected to the inlet end of the dyeing kettle, a valve III is arranged on the connecting pipeline from the outlet end of the dyeing kettle to the inlet end of the condenser, and a valve IV is arranged on the connecting pipeline from the outlet end of the dyeing kettle to the inlet end of the primary separating device.
Has a CO2The outlet end of the storage tank is connected with the inlet end of a delivery pump, and the outlet end of the delivery pump is connected with the CO2The circulating storage tank is connected.
Further, the control unit comprises a temperature sensor, a pressure gauge, a flowmeter, a liquid level meter, an electrical system and a PLC control system; the public module also comprises a safety alarm detection unit, and the safety alarm detection unit consists of an oxygen sensor and a multi-channel controller.
Preferably, the dyeing kettle comprises a loose fiber dyeing storage frame, a cheese dyeing creel and a grey cloth dyeing support; the loose fiber dyeing storage frame and the cheese dyeing creel are of vertical structures, and the grey cloth dyeing support is of a horizontal structure. The fluid inlet of the grey cloth dyeing support adopts a labyrinth type mechanical sealing device and a quick opening part, a magnetic block is connected to a small magnetic motor driving shaft arranged on the quick opening part, a magnetic driving block is arranged at the tail end of the grey cloth dyeing support and is connected with the magnetic block on the small magnetic motor driving shaft, and the rotating speed of the small magnetic motor is 5-10 revolutions per minute.
Still further, as shown in fig. 2, the dye kettle comprises a dye kettle tank body and a dye bin 1 therein, the dye bin 1 comprises a shell, a top cover and a chassis, and an airflow inlet is arranged on the chassis. The dyeing cabin 1 comprises a bottom cylindrical section, a bottom conical section and a cylindrical dyeing cabin main body section which are sequentially connected from bottom to top. A current equalizing functional area, an oligomer separating functional area, a dye storage functional area 4 and a molten dye temporary storage functional area are arranged in the dye bin 1 from bottom to top in a layered mode, and magnetic ring sealing is adopted among the functional areas. The bottom layer partition board between each functional zone is the micropore filter, and the micropore aperture of micropore filter is 25 microns, satisfies the dyestuff of fine powder and can not leak, also can not cause the jam because of the impurity in the dyestuff.
Specifically, the method comprises the following steps: the flow equalizing function area comprises a flow equalizing plate 2 arranged in a bottom end conical section, and a plurality of flow dividing holes are uniformly distributed on the flow equalizing plate 2; the oligomer separation functional zone is a microporous material layer (preferably a volcanic rock particle layer 3 with rough surface and opening rate not less than 70%) for adsorbing oligomers, wherein ethylene terephthalate monomers and dimers in a dissolved state collide with each other on the volcanic rock particle layer 3 with rough surface to form trimers and polymers, and solidification and adsorption are carried out to complete separation of oligomers). The dye storage functional area 4 comprises a grid bin arranged above the volcanic rock particle layer 3, and the grid bin is of an integrated structure made of metal porous filter materials through sintering. The above-mentioned molten dye temporary storage function includes a filament mass (preferably a steel ball layer 5) or a floc uniformly densely arranged on the dye storage function. The flow equalizing plate 2 is provided with at least two layers which are arranged in parallel at intervals; the dye storage functional area 4 is at least provided with two layers which are arranged in parallel at intervals, the thickness of each layer is less than 3 cm, and the area of each grid plane is not more than 2 square centimeters. The steel wire ball layers 5 are uniformly and densely distributed on each dye storage functional area 4, and the molten dye or the auxiliary agent is brought to the molten dye temporary storage functional area by carbon dioxide fluid and is adsorbed and distributed on the steel wire ball layers 5 with large surface areas. The thickness of the temporary storage area of the fused dye is equal to or more than the thickness of a single layer of the functional area 4 of the dye storage, and the single layer of the functional area 4 of the dye storage and the temporary storage area of the fused dye are distributed in 1/1 intervals.
Further, above-mentioned dye bin 1 still include with cylindric dye bin main part section upper end be connected the upper end toper section and with the upper end drum section that upper end toper section is connected sets up the venthole on the upper end drum section lateral wall, sets up impurity filtering function district around the upper end drum section, and impurity filtering function district is the yarn layer 6 of winding in the upper end drum section, and yarn layer 6 covers on the venthole. The winding density of yarn layer 6 is slightly greater than the winding density of the dyed object in the dyeing kettle, so that the blockage phenomenon does not occur while the good filtering effect is ensured, and the yarn layer 6 can be repeatedly utilized.
The dyeing kettle can be of a vertical or horizontal structure, the dyeing bin 1 is arranged in the dyeing kettle, the size of the dyeing bin depends on the size of the dyeing kettle, and the outer wall of the dyeing bin 1 is tightly attached to the inner wall of the dyeing kettle. The periphery of the dyeing bin 1 is provided with a sealing steel plate, and the fluid can only pass through the dyeing bin 1 when flowing through the dyeing kettle in the circulating process of the fluid, so that the fluid is enabled to carry out the dye in a molten state to the maximum extent.
The heat source of the supercritical carbon dioxide anhydrous dyeing system can be any one of steam heating, heat conduction oil heating or electric heating.
The invention discloses a specific using method of a supercritical carbon dioxide anhydrous dyeing system, which comprises the following steps:
liquid CO2Inputting: from CO2The storage tank is pumped to CO by a delivery pump2Circulating the storage tank;
deoiling: circulating pump → valve II → dyeing kettle → valve IV → circulating pump → dyeing kettle → first stage separation device → second stage separation device → condenser → CO2Circulating the storage tank;
dyeing/de-oligomer process: circulating pump → valve I → dyeing kettle → valve IV → circulating pump;
cooling, filtering, heating and removing floating color: circulating pump → valve I → dyeing kettle → valve III → cooler → filter → heat exchanger → circulating pump → dyeing kettle → cooler → filter → heat exchanger;
the recovery process comprises the following steps: dye kettle → primary separation device → secondary separation device → condenser → CO2The storage tank is circulated.
In each process, the corresponding valve is opened or closed according to different requirements.
The invention relates to a specific embodiment of a dyeing method using the supercritical carbon dioxide anhydrous dyeing system, which comprises the following steps in sequence:
deoiling, dyeing/oligomer removing, cooling, filtering, heating and color floating removing, and separating and recycling.
Specifically, the method comprises the following steps: the deoiling procedure comprises the following steps: removing oil agent on the dyed object by using the extraction function of supercritical carbon dioxide; the dyed materials comprise chemical fibers, chemical fiber cheese and chemical fiber fabrics;
the dyeing oligomer-removing step: an adsorption filtering device is arranged at a carbon dioxide fluid outlet of the dyeing kettle, and oligomer monomers dissolved in the carbon dioxide fluid are forced to pass through the adsorption filtering device along with the dyeing process, so that the oligomer is separated out through adsorption and collision;
the step of cooling, filtering, heating and removing the floating color comprises the following steps: the dyeing process temperature is 120-140 ℃, the system starts water cooling and cooling after dyeing is finished, the temperature of the carbon dioxide fluid is cooled to 50-130 ℃, the residual dye in the carbon dioxide fluid is condensed and filtered out by a filter, the filtered pure carbon dioxide fluid enters a heat exchanger to be heated and heated to the dyeing process temperature, and the dye in the carbon dioxide fluid is thoroughly separated after 3-6 cooling, filtering and heating cycles are circulated in the dyeing system.
The separation and recovery step: after the dye in the carbon dioxide fluid is completely separated, the carbon dioxide fluid is separated and recovered.
The dye used in the dyeing step may be a dye dissolved in carbon dioxide for dyeing, or may be another chemical product dissolved in carbon dioxide and absorbed by the material to be dyed.
the specific process for dyeing the polyester filament yarn bobbin yarn comprises the following steps:
（1） CO2storage tank storing liquid CO2Liquid CO is pumped by a delivery pump2Transport to CO2Circulating storage tank (liquid level up to CO)2The transfer pump is turned off and delivery is stopped at recycle tank 2/3).
(2) Starting the low-temperature booster pump to pump CO2Circulating liquid CO in a storage tank2Pumped into the dyeing system.
(3) And starting heating, starting a circulating pump at the same time, and removing the oil agent on the dyed object of the polyester filament yarn cone yarn by utilizing the extraction function of supercritical carbon dioxide after the temperature is raised to the temperature required by the deoiling process. And starting a separation and recovery unit to separate the oil from the carbon dioxide, recovering clean carbon dioxide, and simultaneously starting a low-temperature booster pump to pump new carbon dioxide into the system.
(4) And after the oil agent on the polyester filament cheese is completely removed, closing the separation and recovery unit and the low-temperature booster pump, and continuously heating to the dyeing process temperature of 120 ℃ to perform the dyeing process. Meanwhile, an adsorption filtering device arranged at the outlet of the carbon dioxide fluid of the dyeing kettle is used for filtering and separating the oligomer dissolved in the carbon dioxide fluid.
(5) And after the dyeing process is finished, starting water cooling to cool the carbon dioxide fluid to 80 ℃, condensing the residual dye in the carbon dioxide fluid and filtering the dye by a filter. And (3) heating the filtered pure carbon dioxide fluid in a heating heat exchanger to 120 ℃ of the dyeing process temperature, and circulating the pure carbon dioxide fluid in a dyeing system for 5 cooling, filtering and heating periods to completely separate the dye in the carbon dioxide fluid.
(6) After the dye in the carbon dioxide fluid is thoroughly filtered and separated, the heating and circulating pump is closed, the separation and recovery unit is started, and the clean carbon dioxide fluid after dyeing is recovered to CO2The storage tank is circulated.
the specific process for dyeing the terylene grey cloth comprises the following steps:
（1） CO2storage tank storing liquid CO2Liquid CO is pumped by a delivery pump2Transport to CO2Circulating storage tank (liquid level up to CO)2The transfer pump is turned off and delivery is stopped at recycle tank 2/3).
(2) Starting the low-temperature booster pump to pump CO2Circulating liquid CO in a storage tank2Pumped into the dyeing system.
(3) And starting heating, starting a circulating pump at the same time, and removing the oil agent on the polyester grey cloth by utilizing the extraction function of the supercritical carbon dioxide after the temperature is raised to the temperature required by the deoiling process. And starting a separation and recovery unit to separate the oil from the carbon dioxide, recovering clean carbon dioxide, and simultaneously starting a low-temperature booster pump to pump new carbon dioxide into the system.
(4) And after the oil agent on the polyester grey cloth is completely removed, closing the separation and recovery unit and the low-temperature booster pump, and continuously heating to the dyeing process temperature of 120 ℃ to perform a dyeing process. Meanwhile, an adsorption filtering device arranged at the outlet of the carbon dioxide fluid of the dyeing kettle is used for filtering and separating the oligomer dissolved in the carbon dioxide fluid.
(5) And after the dyeing process is finished, starting water cooling to cool the carbon dioxide fluid to 80 ℃, condensing the residual dye in the carbon dioxide fluid and filtering the dye by a filter. And (3) heating the filtered pure carbon dioxide fluid in a heating heat exchanger to 120 ℃ of the dyeing process temperature, and circulating the pure carbon dioxide fluid in a dyeing system for 5 cooling, filtering and heating periods to completely separate the dye in the carbon dioxide fluid.
(6) After the dye in the carbon dioxide fluid is thoroughly filtered and separated, the heating and circulating pump is closed, the separation and recovery unit is started, and the clean carbon dioxide fluid after dyeing is recovered to CO2The storage tank is circulated.
the specific process for dyeing the polyester loose fibers comprises the following steps:
（1） CO2storage tank storing liquid CO2Liquid CO is pumped by a delivery pump2Transport to CO2Circulating storage tank (liquid level up to CO)2The transfer pump is turned off and delivery is stopped at recycle tank 2/3).
(2) Starting the low-temperature booster pump to pump CO2Circulating liquid CO in a storage tank2Pumped into the dyeing system.
(3) And starting heating, starting a circulating pump at the same time, and removing the oil agent on the polyester loose fibers by utilizing the extraction function of the supercritical carbon dioxide after the temperature is raised to the temperature required by the oil removal process. And starting a separation and recovery unit to separate the oil from the carbon dioxide, recovering clean carbon dioxide, and simultaneously starting a low-temperature booster pump to pump new carbon dioxide into the system.
(4) And after the oil agent on the polyester loose fiber is completely removed, closing the separation and recovery unit and the low-temperature booster pump, and continuously heating to the dyeing process temperature of 120 ℃ to perform the dyeing process. Meanwhile, an adsorption filtering device arranged at the outlet of the carbon dioxide fluid of the dyeing kettle is used for filtering and separating the oligomer dissolved in the carbon dioxide fluid.
(5) And after the dyeing process is finished, starting water cooling to cool the carbon dioxide fluid to 80 ℃, condensing the residual dye in the carbon dioxide fluid and filtering the dye by a filter. And (3) heating the filtered pure carbon dioxide fluid in a heating heat exchanger to 120 ℃ of the dyeing process temperature, and circulating the pure carbon dioxide fluid in a dyeing system for 5 cooling, filtering and heating periods to completely separate the dye in the carbon dioxide fluid.
(6) After the dye in the carbon dioxide fluid is thoroughly filtered and separated, the heating and circulating pump is closed, the separation and recovery unit is started, and the clean carbon dioxide fluid after dyeing is recovered to CO2The storage tank is circulated.
the specific process for dyeing the nylon cheese comprises the following steps:
（1） CO2storage tank storing liquid CO2Liquid CO is pumped by a delivery pump2Transport to CO2Circulating storage tank (liquid level up to CO)2The transfer pump is turned off and delivery is stopped at recycle tank 2/3).
(2) Starting the low-temperature booster pump to pump CO2Circulating liquid CO in a storage tank2Pumped into the dyeing system.
(3) And starting heating, starting a circulating pump at the same time, and removing the oiling agent on the nylon cheese by utilizing the extraction function of supercritical carbon dioxide after the temperature is raised to the temperature required by the oil removal process. And starting a separation and recovery unit to separate the oil from the carbon dioxide, recovering clean carbon dioxide, and simultaneously starting a low-temperature booster pump to pump new carbon dioxide into the system.
(4) And after the oil on the nylon cheese is completely removed, closing the separation and recovery unit and the low-temperature booster pump, and continuously heating to the dyeing process temperature of 120 ℃ to perform a dyeing process. Meanwhile, an adsorption filtering device arranged at the outlet of the carbon dioxide fluid of the dyeing kettle is used for filtering and separating the oligomer dissolved in the carbon dioxide fluid.
(5) And after the dyeing process is finished, starting water cooling to cool the carbon dioxide fluid to 85 ℃, condensing the residual dye in the carbon dioxide fluid and filtering the dye by a filter. And (3) heating the filtered pure carbon dioxide fluid in a heating heat exchanger to 120 ℃ of the dyeing process temperature, and circulating the pure carbon dioxide fluid in a dyeing system for 5 cooling, filtering and heating periods to completely separate the dye in the carbon dioxide fluid.
(6) After the dye in the carbon dioxide fluid is thoroughly filtered and separatedClosing the heating and circulating pump, starting the separation and recovery unit, and recovering the dyed clean carbon dioxide fluid to CO2The storage tank is circulated.
The finished product dyed by the embodiment can meet the requirements of relevant national standards on the color fastness to washing and rubbing.
It is understood that the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and those skilled in the art should also make various changes, modifications, additions or substitutions within the spirit and scope of the present invention.
Claims (10)
1. The supercritical carbon dioxide anhydrous dyeing system is characterized by comprising a dyeing module and a public module, wherein the dyeing module comprises a dyeing unit and a filtering unit, the dyeing unit comprises a dye kettle, a dyeing kettle, a circulating pump and a connecting pipeline, and the filtering unit comprises a cooler, a filter and a heat exchanger; the public module comprises a carbon dioxide storage and conveying unit, a refrigerating unit, a separation and recovery unit and a control unit, wherein the carbon dioxide storage and conveying unit comprises a CO2 circulating storage tank and a low-temperature booster pump; the refrigerating unit comprises a refrigerant tank, a refrigerating compressor, a refrigerant pump, a cold water pump, a water cooling tower and a condenser; the dyeing module is characterized in that at least one dyeing module is arranged on one common module, one dyeing module is connected with the common module through a connecting pipeline, and the rest dyeing modules are sequentially connected in parallel.
2. The supercritical carbon dioxide anhydrous dyeing system according to claim 1, wherein the separation and recovery unit comprises a primary separation device and a secondary separation device, a connecting pipeline led out from the outlet end of the dye kettle is sequentially connected in series with the dyeing kettle, the cooler, the filter, the heat exchanger and the circulating pump and then connected to the inlet end of the dye kettle to form a small circulation, the cooler is cooled by external cooling water, and the heat exchanger is heated by heat-conducting oil; the other connecting pipeline led out from the outlet end of the dyeing kettle is connected with the primary separation device and the secondary separation deviceDevice, condenser, CO2The circulating storage tank and the low-temperature booster pump are sequentially connected in series and then connected to the inlet end of the dye kettle to form a large circulation; the condenser in the public module is connected with the refrigeration compressor, the refrigeration compressor leads out two loops, one loop is formed by connecting the refrigeration compressor in series with a water cooling tower and a cold water pump, and the other loop is formed by connecting the refrigeration compressor in series with a refrigerant tank and a refrigerant pump.
3. The anhydrous supercritical carbon dioxide dyeing system according to claim 2, wherein two connecting lines lead out from the outlet end of the circulating pump, wherein a valve i is arranged on the connecting line connected to the inlet end of the dyeing kettle, a valve ii is arranged on the connecting line connected to the inlet end of the dyeing kettle, a valve iii is arranged on the connecting line from the outlet end of the dyeing kettle to the inlet end of the condenser, and a valve iv is arranged on the connecting line from the outlet end of the dyeing kettle to the inlet end of the primary separation device.
4. The supercritical carbon dioxide anhydrous dyeing system according to any one of claims 1 to 3, characterized by a CO2The outlet end of the storage tank is connected with the inlet end of a delivery pump, and the outlet end of the delivery pump is connected with the CO2The circulating storage tank is connected.
5. The supercritical carbon dioxide anhydrous dyeing system according to any one of claims 1 to 3, characterized in that the control unit comprises a temperature sensor, a pressure gauge, a flow meter, a liquid level meter, an electrical system and a PLC control system; the public module also comprises a safety alarm detection unit, and the safety alarm detection unit consists of an oxygen sensor and a multi-channel controller.
6. The supercritical carbon dioxide anhydrous dyeing system according to any one of claims 1 to 3, characterized in that the dyeing kettle comprises a loose fiber dyeing storage frame, a cheese dyeing creel and a grey cloth dyeing support; the loose fiber dyeing storage frame and the cheese dyeing creel are of vertical structures, the grey cloth dyeing support is of a horizontal structure, a fluid inlet of the grey cloth dyeing support adopts a labyrinth mechanical sealing device and a quick opening part, a small magnetic motor driving shaft arranged on the quick opening part is connected with a magnetic block, and the tail end of the grey cloth dyeing support is provided with a magnetic driving block and is connected with the magnetic block on the small magnetic motor driving shaft.
7. The supercritical carbon dioxide anhydrous dyeing system according to any one of claims 1 to 3, characterized in that the dye kettle comprises a dye kettle tank body and a dye bin therein, the dye bin comprises a shell, a top cover and a base plate, an air flow inlet is arranged on the base plate, the dye bin comprises a bottom cylindrical section, a bottom conical section and a cylindrical dye bin main body section which are sequentially connected from bottom to top, a flow equalizing functional area, an oligomer separating functional area, a dye storing functional area and a molten dye temporary storage functional area are arranged in the dye bin layer by layer from bottom to top, magnetic rings are used for sealing among the functional areas, and a bottom partition plate between the functional areas is a microporous filter plate; the flow equalizing functional area comprises a flow equalizing plate arranged in the bottom end conical section, a plurality of flow dividing holes are uniformly distributed on the flow equalizing plate, and the oligomer separation functional area is a microporous material layer which is used for adsorbing oligomers and has a rough surface; the dye storage functional area comprises a grid bin arranged above the microporous material layer, and the grid bin is an integral structure made of a metal porous filtering material through sintering; the molten dye temporary storage functional area comprises filament clusters which are uniformly and densely distributed on the dye storage functional area.
8. The supercritical carbon dioxide anhydrous dyeing system according to claim 6, characterized in that the dye kettle comprises a dye kettle tank body and a dye bin therein, the dye bin comprises a shell, a top cover and a chassis, an airflow inlet is arranged on the chassis, the dye bin comprises a bottom cylindrical section, a bottom conical section and a cylindrical dye bin main body section which are sequentially connected from bottom to top, a flow equalizing function region, an oligomer separation function region, a dye storage function region and a molten dye temporary storage function region are arranged in the dye bin layer by layer from bottom to top, magnetic rings are adopted for sealing among the function regions, and a bottom partition plate among the function regions is a microporous filter plate; the flow equalizing functional area comprises a flow equalizing plate arranged in the bottom end conical section, a plurality of flow dividing holes are uniformly distributed on the flow equalizing plate, and the oligomer separation functional area is a microporous material layer which is used for adsorbing oligomers and has a rough surface; the dye storage functional area comprises a grid bin arranged above the microporous material layer, and the grid bin is an integral structure made of a metal porous filtering material through sintering; the molten dye temporary storage functional area comprises filament clusters which are uniformly and densely distributed on the dye storage functional area.
9. A dyeing method using the supercritical carbon dioxide anhydrous dyeing system according to any one of claims 1 to 8, characterized in that the dyeing method comprises the following steps carried out in sequence:
deoiling, dyeing/oligomer removing, cooling, filtering, heating and color floating removing, and separating and recycling.
10. The dyeing method of the supercritical carbon dioxide anhydrous dyeing system according to claim 9, characterized in that the degreasing process: removing oil agent on the dyed object by using the extraction function of supercritical carbon dioxide; the dyed materials comprise chemical fibers, chemical fiber cheese and chemical fiber fabrics;
the dyeing oligomer removing procedure comprises the following steps: an adsorption filtering device is arranged at a carbon dioxide fluid outlet of the dyeing kettle, and oligomer monomers dissolved in the carbon dioxide fluid are forced to pass through the adsorption filtering device along with the dyeing process, so that the oligomer is separated out through adsorption and collision;
the temperature reduction, filtration and temperature rise floating color removal process comprises the following steps: the dyeing process temperature is 120-;
the separation and recovery step: when the dye in the carbon dioxide fluid is completely separated, the carbon dioxide fluid is separated and recovered.
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| CN114606692A (en) * | 2022-03-25 | 2022-06-10 | 东华大学 | Method for improving solubility and dissolution rate of dyes in supercritical carbon dioxide fluid |
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