WO2021121409A1

WO2021121409A1 - Pulse-type supercritical carbon dioxide printing and dyeing device

Info

Publication number: WO2021121409A1
Application number: PCT/CN2020/137761
Authority: WO
Inventors: 杨景峰
Original assignee: 上海复璐帝流体技术有限公司
Priority date: 2019-12-18
Filing date: 2020-12-18
Publication date: 2021-06-24
Also published as: CN211394932U

Abstract

Disclosed in the present utility model is a pulse-type supercritical carbon dioxide printing and dyeing device, comprising: a CO₂ storage tank, a three-primary-color tank, a dye tank, a pulse-type generator, a dyeing kettle, a dye collection tank, a pressure reduction cooling unit, and an extraction separation unit, wherein the CO₂ storage tank is connected to the dye tank by means of the three-primary-color tank after sequentially passing through a filtering unit, a drying unit, a heating unit, and a pressurizing unit; the dye tank is connected to the dyeing kettle by means of an auxiliary tank, a flowmeter, and a plurality of parallel-connected pulse-type injectors in sequence; each of the pulse-type injectors is separately connected to a plurality of liquid inlet holes in each section of the dyeing kettle; each section of the dyeing kettle is provided with a dual-core ultrasonic generation device and a bidirectional circulating pump; and the bottom of the dyeing kettle is connected to the dye tank and the dye collection tank by means of pipelines. The optimal dye liquor conveying condition can be implemented by adopting pulse type conveying; the printing and dyeing uniformity and the printing and dyeing efficiency are improved; and a printing and dyeing process is environment-friendly, clean in production, good in economic benefits, and remarkable in environmental benefits.

Description

Pulse type supercritical carbon dioxide printing and dyeing device

Technical field

The utility model relates to the technical field of printing and dyeing, in particular to a pulsed supercritical carbon dioxide printing and dyeing device.

Background technique

The existing supercritical carbon dioxide printing and dyeing process is only semi-continuous, and the dyeing kettle does not have thermal insulation measures, resulting in the loss of a large amount of heat in the process; in the dyeing process, only a one-way circulation pump is configured, resulting in the uniformity of product dyeing. Certain problems; the existing dyeing auxiliaries do not achieve the best dyeing aid effect; the existing supercritical carbon dioxide printing and dyeing process has not been effectively combined with the effect of ultrasound; the remaining dye liquor has not been recycled for continuous production Utilizing these factors causes the current supercritical carbon dioxide printing and dyeing process to be in a state of low efficiency, large energy consumption, high cost, and low benefit, and there are problems of substandard product uniformity and lengthy equipment. Therefore, it is necessary to develop a printing and dyeing process that can realize environmental protection, clean production, recycling, high yield and low cost.

Utility model content

The technical problem to be solved by the utility model is: in view of the above-mentioned defects in the prior art, a pulsed supercritical carbon dioxide printing and dyeing device is proposed.

In order to achieve the above purpose, the present utility model adopts the following technical solutions:

The utility model provides a pulsed supercritical carbon dioxide printing and dyeing device, which includes: a CO2 storage tank, a three-primary color tank, a dye tank, a pulse generator, a dyeing kettle, a dye collection tank, a decompression cooling unit and an extraction separation unit, in which:

The CO2 storage tank is connected to the dye tank via the three primary color tanks through a pipeline through a filter unit, a drying unit, a heating unit, and a pressurizing unit, so as to convert the carbon dioxide in the CO2 storage tank after pressurization and heating treatments. It is supercritical carbon dioxide, and the supercritical carbon dioxide is mixed with the three primary color dyes in the three primary color tanks in a certain proportion in the dye tank to form a dye solution;

The dye tank is connected to the dyeing tank through a pipeline via an auxiliary tank, a flow meter, and a number of pulse injectors connected in parallel, and each pulse injector is connected to the top and/or bottom of each section of the dyeing tank in turn. A number of liquid inlet holes are arranged, which are used to send the dye solution into each section of the dyeing kettle by pulse injection through the pulse injector to dye the spindles from the end of the spindle; each section of the dyeing kettle A dual-core ultrasonic generating device and a two-way circulation pump are provided on the two-way circulation pump. Both ends of the two-way circulation pump are connected to the pulse syringe and the dyeing kettle with Y-shaped connectors, and the two Y-shaped connectors are located in each section. The liquid inlet holes at both ends of the bottom of the dyeing kettle;

The bottom of the dyeing tank is connected to the dye tank through a pipe to return the remaining dye liquor discharged from the dyeing tank to the dye tank for recycling; or the bottom of the dyeing tank is connected to the dye collection tank through a pipe to remove The remaining dye liquor after dyeing in the dyeing kettle is collected in the dye collection tank, and after separation and purification is processed into liquid carbon dioxide and dye, it is transported as liquid carbon dioxide raw material and dye raw material to the CO2 storage tank and dye tank respectively through pipelines Recycle or store for future use.

Further, the bottom of the dyeing kettle is connected to the decompression cooling unit through the dye collecting tank through a pipeline, so as to collect the remaining dye liquor after dyeing in the dyeing kettle in the dye collecting tank and pass through the dye collecting tank. The decompression cooling unit decompresses and separates the remaining dye liquor.

Further, the top end of the decompression cooling unit is connected to the CO2 storage tank through the purification unit, the filter unit and the drying unit through a pipeline, so that the separated carbon dioxide gas is sent to the CO2 storage tank for recycling.

Further, the bottom end of the decompression cooling unit is connected to the extraction separation unit through a pipe to extract the separated dye solution, and the extracted dye is sent to the dye tank for recycling and/or after extraction. The auxiliary agent is sent to the auxiliary agent tank for recycling.

Further, the dyeing kettle is composed of a pipe of 24-25 meters, and is covered with a thermal insulation layer.

Further, the dyeing kettle is divided into four sections along its length direction, and each section of the dyeing kettle is provided with the pulse injector, the ultrasonic generator and the two-way circulation pump.

Further preferably, a liquid inlet is respectively opened at 1000 mm, 3000 mm, and 5000 mm from the ingot outlet end of each section of the dyeing kettle, and the liquid inlet is connected to the pulse injector through a pipe.

Further preferably, drainage holes are respectively opened at 375mm, 625mm, 875mm, and 1125mm from the ingot outlet end of each section of the dyeing kettle, and the drainage hole is connected to the dye tank and the dye collection tank through a pipe.

More preferably, the liquid discharge hole and the liquid inlet hole both have a large and small head structure, and both are composed of an upper hole and a lower hole.

Further, the axis angle between the two ports in the double port direction on the Y-shaped port is 90°.

Compared with the prior art, the utility model adopts the above technical scheme and has the following technical effects:

(1) The pulsed supercritical carbon dioxide printing and dyeing device is equipped with a two-way circulation pump to complete a set of forward and reverse cycles in 4-5 minutes to improve the uniformity of product dyeing; equipped with a pulse injection machine, the value is 0.5-1 In minutes, complete a set of pulsed dye injection at the upper and lower ends at the same time; at the same time, the same frequency ultrasound is added to increase the activity of dye molecules and dye-assisting molecules, speed up the diffusion and adsorption of dye molecules, and improve dyeing efficiency;

(2) The pulsed supercritical carbon dioxide printing and dyeing device adopts Y-shaped interface to connect pulse injection machine, two-way circulation pump and dyeing kettle at the same time. Regardless of whether the two-way circulation pump circulates in the positive or negative direction, it can speed up the fluidity and fluidity of the dye solution. Improve the uniformity of the dye solution injected by the pulse injection machine and the original dye solution in the dyeing kettle, prevent color difference, thereby improve the uniformity of dyeing and improve product quality;

(3) The pulsed supercritical carbon dioxide printing and dyeing device can make the dyeing process faster by adding auxiliary agents to the dissolved dye solution, and the spindle has a stronger adsorption of dye; it can successfully dye a spindle and spindle within 30 minutes Enter the product collection trolley from the ingot end at an interval of about 18 seconds;

(4) In this pulsed supercritical carbon dioxide printing and dyeing device, the remaining dye solution collector is added at the outlet end, and the remaining dye solution collector is connected to the remaining dye solution collector by opening holes at 375mm, 625mm, 875mm, and 1125mm from the outlet end. , Separate supercritical carbon dioxide from dyes and auxiliaries through a decompression separation device, separate dyes and auxiliaries through extraction, and then separately purify and dry the supercritical carbon dioxide, dyes and auxiliaries, and then circulate them to the raw material warehouse; Realize green, clean production, recycling, high-yield, low-cost printing and dyeing process using supercritical carbon dioxide;

(5) The existing method of delivering the dye solution is pressure conveying, and the pulsed supercritical carbon dioxide printing and dyeing device adopts pulse conveying. The pulse frequency is based on different printed and dyed materials, different periods of time during the printing and dyeing process, and the dyeing kettle. It varies from section to section and is precisely adjusted from time to time to achieve the best dye liquor delivery condition; pulsed conveying is also conducive to increasing the chaos of the dye liquor in the dyeing kettle, and at the same time strengthens the convection of the dye liquor, which can improve The uniformity of printing and dyeing and the efficiency of printing and dyeing;

(6) The pressure of the pulsed supercritical carbon dioxide printing and dyeing device is reduced by 30% to 46%, which is 25% to 33% lower than the printing and dyeing temperature of ordinary equipment, which greatly reduces the cost of equipment and heating; and Compared with the existing process equipment, the printing and dyeing efficiency has been increased by 16% to 33%; due to the dual-core ultrasonic configuration, the dyeing can be more uniform, which greatly reduces the color difference between the inner and outer coils, and also improves the color fastness of the fabric. Up to level 5.

Description of the drawings

Figure 1 is a schematic structural diagram of a pulsed supercritical carbon dioxide printing and dyeing device of the utility model;

Figure 2 is a schematic diagram of the structure of the ingot end of a 1/4 dyeing kettle in a pulsed supercritical carbon dioxide printing and dyeing device of the utility model;

Fig. 3 is a partial enlarged schematic diagram of part A in the ingot end of the dyeing kettle shown in Fig. 2;

Figure 4 is a schematic diagram of the structure of the output end of the dyeing kettle in a pulsed supercritical carbon dioxide printing and dyeing device of the utility model;

Figure 5 is a partial enlarged schematic view of the structure of part B in the outlet end of the dyeing kettle shown in Figure 2;

Figure 6 is a schematic diagram of a Y-shaped interface in a pulsed supercritical carbon dioxide printing and dyeing device of the utility model;

Figure 7 is a schematic structural diagram of a yarn tube in a pulsed supercritical carbon dioxide printing and dyeing device of the utility model;

Figure 8 is a graph showing the diffusion curve of dyes in fibers in a pulsed supercritical carbon dioxide printing and dyeing process of the utility model.

Detailed ways

Hereinafter, the present utility model will be described in detail and concretely through specific embodiments, so as to better understand the present utility model, but the following embodiments do not limit the scope of the present utility model.

Example 1

Please refer to Figure 1, this embodiment provides a pulsed supercritical carbon dioxide printing and dyeing device, including: CO ₂ storage tank, three primary color tank, dye tank, pulse generator, dyeing kettle, dye collection tank, decompression cooling unit And an extraction separation unit, the three primary color tanks are composed of a red tank, a yellow tank and a blue tank arranged in parallel, and the red, yellow and blue tanks are respectively equipped with three primary color dyes of red, yellow and blue, and the three primary color dyes of red, yellow and blue are arranged according to Need to install a certain proportion of dye solution mixed with supercritical carbon dioxide to form a specific color. The dyeing kettle is composed of a pipe of 24-25 meters, covered with a thermal insulation layer; and is divided into four sections along its length, and each section of the dyeing kettle is provided with the pulse injector and ultrasonic Generator and two-way circulation pump.

In this implementation, please refer to FIG. 1, the CO ₂ storage tank is connected to the dye tank via the three primary color tanks through the pipeline, the filter unit, the drying unit, the heating unit, and the pressurizing unit in order, to remove the CO ₂ The carbon dioxide in the storage tank is pressurized and heated to convert into supercritical carbon dioxide, and the supercritical carbon dioxide is mixed with the three primary color dyes in the three primary color tanks in a certain proportion to form a dye solution.

In this implementation, please refer to Figure 1. The dye tank is connected to the dyeing tank through a pipeline via an auxiliary tank, a flow meter and a number of pulse-type syringes connected in parallel, and each pulse-type syringe is connected to the dyeing tank. The several liquid inlet holes arranged in sequence at the top and/or bottom of each section of the dyeing kettle are used to send the dye solution into each section of the dyeing kettle in a pulsed injection manner through the pulse injector. The spindle at the spindle end is dyed; each section of the dyeing kettle is provided with a dual-core ultrasonic generator and a two-way circulation pump, and the two ends of the two-way circulation pump are respectively connected to the pulse injector and the dyeing kettle through Y-shaped interfaces, And the two Y-shaped joints are respectively located at the liquid inlet holes at the two ends of the bottom of each section of the dyeing kettle.

In this implementation, please refer to FIG. 1, the bottom of the dyeing tank is connected to the dye tank through a pipe to return the remaining dye liquor discharged from the dyeing tank to the dye tank for recycling; or the bottom of the dyeing tank The dye collection tank is connected through a pipeline to collect the remaining dye liquor after dyeing in the dyeing tank in the dye collection tank, and after separation and purification is processed into liquid carbon dioxide and dye, they are used as liquid carbon dioxide raw materials and dye raw materials, respectively It is transported to the CO ₂ storage tank and the dye tank through a pipeline for recycling or storage for use.

In this implementation, please refer to FIG. 1, the bottom of the dyeing tank is connected to the decompression cooling unit through the dye collection tank through a pipe, so as to collect the remaining dye liquor after dyeing in the dyeing tank in the dyeing tank. In the dye collection tank, the remaining dye liquor is decompressed and separated through the decompression cooling unit; the top of the decompression cooling unit is connected to the purification unit, the filter unit, and the drying unit through a pipeline. CO ₂ storage tank, to send the separated carbon dioxide gas into the CO ₂ storage tank for recycling; and the bottom end of the reduced pressure cooling unit is connected to the extraction separation unit through a pipeline to carry out the separation of the dye liquor In the extraction process, the extracted dye is sent to the dye tank for recycling, and/or the extracted auxiliary is sent to the auxiliary tank for recycling.

Please refer to Figure 2-3, which is a schematic structural diagram of a quarter-length dyeing kettle, and the used dyeing kettle is divided into at least one section along its length. Specifically, the dyeing kettle has a total length of 24-25m and is divided into 4 sections along its length direction. The length L16 of each section of the dyeing kettle is 5000-7000mm, preferably 6000mm, and the outer diameter of each section of the dyeing kettle is R1. It is 220-280mm, preferably 245mm; the inner diameter R2 of each section of the dyeing kettle is 150-210mm, preferably 175mm. The impulse syringes are respectively connected to L11, L13, and L15 from the top and bottom of the dyeing entrance end of each section of the dyeing kettle to have liquid inlet holes in sequence, and the L11 is 800-1200mm away from the entrance end, preferably 1000mm; The L13 is 2800-3200mm away from the entrance end, preferably 3000mm, and the L15 is 400-5200mm away from the entrance end, preferably 5000mm.

As a preferred technical solution, the impulse injector is connected to the top and top positions of the dyeing tank at 1000mm, 3000mm and 5000mm respectively. There are 6 liquid inlet holes in total. The liquid inlet holes are in the structure of small and small heads. The upper hole and the lower hole are formed. The total height R3 of the liquid inlet hole is 30-40mm, preferably 35mm; the height of the upper hole R4 is 20-30mm, preferably 25mm; the diameter R7 of the upper hole is 25 -30mm, preferably 26.1; the upper hole is in the shape of an opening, the opening angle is 60°, and the opening height R8 is 2-3mm, preferably 2.39mm. The height R6 of the lower hole is 8-12 mm, preferably 9 mm; the diameter R5 of the lower hole is 3-8 mm, preferably 6 mm.

As a preferred technical solution, the two ends of the two-way circulation pump are respectively connected to the lower ends of the ingot end L11-1000mm and L15-5000mm of each section of the dyeing kettle, and the two ends of the two-way circulation pump are respectively connected through a Y-shaped interface. It is connected with the pulse type syringe and the dyeing kettle, the two ports of the double port direction on the Y-shaped interface are connected to the bidirectional circulation pump and the pulse type syringe, and the one port of the single port direction on the Y-shaped port is connected to the dyeing tank. The liquid inlet holes at both ends of the bottom of the kettle.

As a preferred technical solution, the pulsed supercritical carbon dioxide printing and dyeing device of this embodiment is only equipped with a one-way circulation pump and continuous dye injection from top to bottom on the current dyeing kettle, which causes certain problems in the uniformity of product dyeing. defect. The dyeing kettle is equipped with 4 two-way circulation pumps in sequence to complete a set of forward and reverse cycles in 4-5 minutes to improve the uniformity of product dyeing; 4 pulse injection machines are equipped with 0.5-1 minutes as the unit Complete a set of pulsed dye injection at the upper and lower ends at the same time; equipped with 4 sets of same-frequency ultrasound to increase the activity of dye molecules and dye-assisting molecules, speed up the diffusion and adsorption process of dye molecules, and improve dyeing efficiency.

Please refer to Figure 1. In the entire dyeing kettle, each section of the dyeing kettle is equipped with the pulse injector, ultrasonic generator and two-way circulation pump, and the four sections of the dyeing kettle are equipped with four two-way circulation pumps. Circulating pumps, so a total of 8 Y-shaped connections need to be added, and 2 are installed on each section of the dyeing kettle. The axis angle between the two ports in the double-port direction on the Y-shaped interface is 90°, the length Y1 of the single-port direction on the Y-shaped interface is 40-60mm, preferably 50mm; the double-port on the Y-shaped interface The length Y2 of the two ports in the direction is 70-90mm, preferably 80mm; the inner diameter Y3 of the three ports on the Y-shaped port is 15-25mm, preferably 20mm; the outer diameter Y4 of the three ports on the Y-shaped port is 20 -30mm, preferably 26mm. The two ports in the double port direction of the Y-shaped port are respectively closely matched with the connecting pipes of the pulse injector and the bidirectional circulating pump in an interference manner. The connecting pipe between the Y-shaped interface and the pulse syringe is equipped with a one-way valve; the connection pipe between the Y-shaped interface and the bidirectional circulating pump is equipped with a bidirectional valve, and the switch of the bidirectional valve is automatically adjusted according to the output direction of the bidirectional circulating pump. .

In this embodiment, please refer to Figure 6, the ports corresponding to the two ports of the Y-shaped port are in the single port direction, and the single port direction of the Y-shaped port is in an interference manner with the 1000mm and 5000mm positions of each section of the dyeing kettle. The lower end of the inlet is tightly fitted, and the use of an interference tight fit can prevent the leakage of high-pressure liquid better than the threaded connection. The biggest advantage of using the Y-shaped interface is that it can connect the pulse syringe and the two-way circulating pump at the same time. Regardless of whether the two-way circulating pump circulates in the positive or negative direction, it can speed up the fluidity of the dye and improve the dye and dye injected by the pulse syringe. The uniformity of the original dyeing solution in the kettle prevents color difference, thereby improving the uniformity of dyeing and improving product quality. It can also reduce the number of openings in the dyeing kettle. At the same time, it can reduce the flow resistance of high-pressure liquid compared with ordinary three-way interfaces. Thereby improving the safety of the equipment, in addition, the Y-shaped interface and the two-way valve can prevent the impact and damage of the two-way circulation pump due to the pulse-injected dye solution, thereby improving the stability and service life of the equipment.

In this embodiment, referring to Figures 3-4, the existing ingot discharge end is not equipped with a residual dye liquor collector, which results in the disadvantages that it is difficult to realize waste recycling and reuse and the cost is high. A remaining dye solution collection tank is added at the outlet end of the dyeing kettle; drain holes are respectively opened at L21, L22, L23, L24 from the bottom of the outlet end of the dyeing kettle, and the L21 is 350-400mm from the outlet end The position is preferably 375mm; the L22 is 600-650mm away from the ingot end, preferably 625mm; the L23 is 850-900mm away from the ingot end, preferably 875mm; the L24 is away from the ingot end The end is at 1100-1150mm, preferably at 1125mm. That is, as a preferred embodiment, the four drain holes are arranged in sequence at the bottom of the dyeing tank at 375mm, 625mm, 875mm, and 1125mm from the end of the spindle, and each of the drain holes is connected to the dye through a pipe. Tank and the dye collection tank. The liquid discharge hole has the same structure as the liquid inlet hole, and both have a large and small head structure. The total height R3 of the drainage hole is 30-40mm, preferably 35mm; the height of the upper hole R4 is 20-30mm, preferably 25mm; the diameter R7 of the upper hole is 25-30mm, preferably 26.1; The upper hole has an opening shape, the opening angle is 60°, and the opening height R8 is 2-3 mm, preferably 2.39 mm. The height R6 of the lower hole is 8-12 mm, preferably 9 mm; the diameter R5 of the lower hole is 3-8 mm, preferably 6 mm.

In this embodiment, as a preferred technical solution, the dyeing kettle is also provided with a pressure gauge, and the pressure gauges are respectively installed at the openings at the upper end 2000mm and 4000mm away from the dyeing inlet end of each section of the dyeing kettle, and the pressure gauge is used for To monitor the pressure change in the dyeing kettle. The dyeing process used in this embodiment can successfully dye a spindle within 30 minutes, and the spindle enters the product collection unit from the end of the spindle at a time interval of about 18 seconds.

The pulsed supercritical carbon dioxide printing and dyeing device provided in this embodiment, in view of the defect that the dyeing kettle has no thermal insulation measures, resulting in the loss of a large amount of heat in the process, a thermal insulation layer is added to the dyeing kettle to reduce the number of printing and dyeing process engineering. The heat is lost and the temperature stability in the printing and dyeing process is ensured, energy consumption is reduced, and the quality and efficiency of printing and dyeing are improved.

Compared with the existing supercritical carbon dioxide printing and dyeing technology, the pulsed supercritical carbon dioxide printing and dyeing device provided in this embodiment has obvious advantages. The best effect that the existing supercritical carbon dioxide printing and dyeing technology can achieve is that the minimum printing and dyeing pressure is about 16-18Mpa, the printing and dyeing pressure of general equipment is 20-30Mpa; the minimum printing and dyeing temperature is about 110℃, and the printing and dyeing temperature of general equipment is 120. ～135℃; Printing and dyeing time is about 35～45 minutes. Compared with the existing ordinary equipment, the pulsed supercritical carbon dioxide printing and dyeing device provided by this embodiment reduces the pressure suffered by 30% to 46%, and reduces the printing and dyeing temperature by 25% to 33% compared with the existing ordinary equipment. It will also greatly reduce equipment costs and heating costs; compared with the existing process equipment, the printing and dyeing efficiency is increased by 16% to 33%. Due to the dual-core ultrasonic configuration, the dyeing can be more uniform, which greatly reduces the color difference between the inner and outer coils, and also improves the color fastness of the fabric up to level 5.

The working principle of the pulsed supercritical carbon dioxide printing and dyeing device is: the liquid carbon dioxide is _{injected from the CO 2} storage tank through the heating unit, the pressurizing unit, the dye tank, the auxiliary tank, and the feeding pump into the dyeing tank through the pulse injector. , Two-way circulation and auxiliaries work together to dye the incoming material from the ingot end, and the dyeing kettle is covered with a thermal insulation layer; after dyeing mature, the ingot leaves from the ingot end and enters the product collection trolley for consignment to the next process The dye liquor discharged from the dyeing tank is returned to the dye tank for recycling; or the discharged dye liquor is separated and purified into liquid carbon dioxide and dye, and then recycled or stored as a liquid carbon dioxide raw material and dye raw material. The printing and dyeing dye conveying device produces no dyeing wastewater and other wastes, and can realize the characteristics of green environmental protection, clean production, good economic benefits, and remarkable environmental benefits, and can realize the purpose of recycling, flowing water production, increasing output, and reducing industrial costs.

Example 2

Please refer to Figure 1, based on the above-mentioned pulsed supercritical carbon dioxide printing and dyeing device, this embodiment provides a pulsed supercritical carbon dioxide printing and dyeing process suitable for printing and dyeing the same product for the first time or continuously printing and dyeing the same product, including the following steps: ( 1) Pass the liquid carbon dioxide from the CO ₂ storage tank through the filter unit, the drying unit, the heating unit and the pressurizing unit in order, after being pressurized and heated, and then converted into supercritical carbon dioxide; (2) The converted supercritical carbon dioxide is passed through separately Mix the red, yellow, and blue dyes into the three primary color tanks, red, yellow, and blue dyes, and then pass them into the dye tank in a certain proportion according to the dyeing requirements of the yarn spindle to form the dye solution; (3) Use a pulse injector to transfer the dye solution Inject the liquid into the dyeing kettle from the top and bottom of the dyeing kettle respectively, and dye the spindles from the end of the spindle under the combined action of the ultrasonic generator and the two-way circulation pump, and the dyeing kettle is surrounded by a thermal insulation layer. After the dyeing is mature, it is sent out from the ingot end and enters the product collection unit for consignment to the next process; (4) The dye liquor discharged from the dyeing tank is not collected by the dye collector, but is directly returned to the dye tank to enter the printing and dyeing cycle for recycling.

In this embodiment, in step (1), the pressure increase unit is used to increase the pressure of carbon dioxide to above 16 MPa; the heating unit needs to heat the temperature of carbon dioxide to above 80°C. That is, the carbon dioxide is converted into supercritical carbon dioxide through the pressurizing unit and the heating unit, the pressurizing unit uses a booster pump, and the heating unit can use a heater.

In this embodiment, step (2) also includes adding a dyeing aid to the dye liquor. The dyeing aid used is suitable for supercritical carbon dioxide printing, and the remaining dye liquor can be used with supercritical carbon dioxide. Oxidation, dye separation, realize recycling.

In this embodiment, the working power of the ultrasonic generator in step (3) is 600W to ultrasonically treat the dye solution and spindles in the dyeing kettle. The ultrasonic generator uses a dual-core ultrasonic generator; in the dyeing kettle Equipped with an ultrasonic generator, it can improve the activity of dye molecules and dye-assisting molecules, speed up the diffusion and adsorption process of dye molecules, and improve dyeing efficiency. In addition, a two-way circulation pump is equipped on the dyeing kettle, which can realize the forward and reverse two-way circulation of the dye in the dyeing kettle, improve the uniformity of product dyeing, and complete a set of forward and reverse circulation processes in 4-5 minutes; and the two-way circulation pump can carry out Adjust the speed, according to different fabrics, the circulation speed of the dyeing liquor can be adjusted. Specifically, a two-way circulation pump is used to circulate the dyeing solution in the dyeing kettle at a speed of 2.4 m/min, and the spindles advance in the dyeing kettle at a rate of 1.2 m/min and perform dyeing.

In this embodiment, the yarn spindle to be dyed in step (3) is heated, swelled and dried before entering the dyeing kettle to improve the dyeing speed and dyeing quality of the dye in the dyeing kettle. In addition, this step (3) also includes heat preservation and heat insulation treatment on the dyeing kettle during the dyeing process. The heat preservation and heat insulation is achieved by setting the heat preservation and heat insulation sleeve in the dyeing kettle. The design of heat preservation and heat insulation can be used in the printing and dyeing process. Reduce heat loss and improve the stability of printing and dyeing temperature, improve economic efficiency, and reduce energy consumption.

Example 3

Please refer to FIG. 1, which is different from the above-mentioned embodiment 2. Based on the above-mentioned pulsed supercritical carbon dioxide printing and dyeing device, this embodiment provides a pulsed supercritical carbon dioxide printing and dyeing process suitable for when printing and dyeing products stop production, including the following steps : (1) The liquid carbon dioxide from the CO ₂ storage tank is sequentially passed through the filter unit, the drying unit, the heating unit and the pressurizing unit, after being pressurized and heated, and then converted into supercritical carbon dioxide; (2) the converted supercritical carbon dioxide Pass the three primary color tanks into the red, yellow, and blue tanks and mix them with red, yellow, and blue dyes, and then pass them into the dye tank in a certain proportion according to the dyeing requirements of the spindles to form the dye solution; (3) Use a pulse injector to mix The dye liquor is injected into the dyeing kettle from the liquid inlet holes at the top and bottom of the dyeing kettle respectively, and dyes the spindles from the end of the spindle under the combined action of the ultrasonic generator and the two-way circulation pump, and the outer periphery of the dyeing kettle is covered with a thermal insulation layer. After dyeing mature, the spindle is sent out from the spindle end and enters the product collection unit for consignment to the next process; (4) Collect the remaining dye through the dye collection tank, and separate the supercritical carbon dioxide, dye and auxiliaries through the decompression cooling unit, and then pass through The extraction method separates the dye and the auxiliary agent, and then the supercritical carbon dioxide, the dye and the auxiliary agent are purified and dried respectively, and then they are recycled and stored separately for later reuse or subsequent unified treatment.

Example 4

Please refer to FIG. 1, which is different from the above-mentioned Embodiment 2. Based on the above-mentioned pulsed supercritical carbon dioxide printing and dyeing device, this embodiment provides a pulse that is suitable for printing and dyeing of the same type of printed and dyed material before and after the change is not large. The supercritical carbon dioxide printing and dyeing process includes the following steps: (1) The liquid carbon dioxide is transferred from the CO ₂ storage tank through the filter unit, the drying unit, the heating unit and the pressurizing unit to supercritical carbon dioxide after being pressurized and heated; (2) Pass the converted supercritical carbon dioxide into the red, yellow, and blue tanks of the three primary color tanks and mix them with red, yellow, and blue dyes, and then pass them into the dye tank in a certain proportion according to the dyeing requirements of the spindles to form dyeing. (3) Use a pulsed syringe to inject the dye solution into the dyeing kettle from the top and bottom inlet holes of the dyeing kettle, and dye the spindles from the ingot end under the combined action of the ultrasonic generator and the two-way circulating pump And there is a thermal insulation layer on the periphery of the dyeing kettle. After the dyeing is mature, the yarn spindle is sent out from the spindle end, and then enters the product collection unit for consignment to the next process; (4) Collect the remaining dye through the dye collection tank, and supercritically through the decompression cooling unit The carbon dioxide, dyes and auxiliaries are separated, and then the dyes and auxiliaries are separated by extraction. After the supercritical carbon dioxide, dyes and auxiliaries are purified and dried respectively, they are purified and dried respectively, and then recycled to the CO ₂ storage tank, Dye tank and auxiliary tank.

Application example 1

Based on the pulsed supercritical carbon dioxide printing and dyeing process and device, this application example provides a process for dyeing synthetic fibers (polyester fabric). As shown in Figure 1, the process consists of six parts to form a complete automated process, including the CO ₂ storage tank part, the pressurized part, the heating part, the dye mixing part, the dual-cycle ultrasonic printing and dyeing part, and the dye circulation part.

When entering the printing and dyeing process, the liquid carbon dioxide _{flows out of the CO 2} storage tank, and sequentially passes through the filter unit, drying unit, heating unit, pressurizing unit, dye tank, auxiliary tank, and feed pump into the dyeing tank through the pulse injector. The pre-heated and dried yarn spindles and the dye injected into the dyeing kettle by pulse are dyed under the combined action of KC-TC01 dual-core ultrasonic and two-way circulating pump, and the outer periphery of the dyeing kettle is covered with a thermal insulation layer. At this time, the pressurizing unit (booster pump) needs to pressurize the carbon dioxide pressure to above 16MPa; the heating unit (heater) needs to heat the carbon dioxide temperature to above 100℃; the supercritical carbon dioxide is respectively passed into the three primary color tanks and the dye is dissolved, and then Into the dye tank to form the dye solution; the auxiliary tank does not need to add any dye, and the dye solution can pass directly through the auxiliary tank; the KC-TC01 dual-core ultrasonic working power is 600W, and the two-way circulation pump transfers the dye solution to 2.4m/min The speed circulates in the dyeing kettle to improve the uniformity of the dye. The spindle advances and dyes in the dyeing kettle at an amplitude of 1.2m/min. After the yarn spindle is dyed and matured, it leaves from the spindle end and enters the product collection unit for consignment to the next process. The remaining dye that flows out is not collected by the dye collector, but is directly returned to the dye tank to enter the printing and dyeing cycle for reuse.

Based on the dyeing process of the synthetic fiber (polyester fabric) of this embodiment, a method for constructing a mass transfer model of the synthetic fiber (polyester fabric) during the printing and dyeing process is provided:

As shown in Figure 8, the fiber center is taken as the axis and the fiber radial direction is taken as the x-axis, a one-dimensional coordinate system. The dye precipitates on the surface of the fiber and then diffuses into the fiber.

The diffusion process of the dye in the fiber follows:

In the formula: C _A -the dye molar concentration at any time and any position in the fiber;

D _AB -the diffusion coefficient of the dye atom in the fiber;

The precipitation process of the dye solution on the fiber surface follows:

N _A ＝k(C _Af -C _A0 ) (2)

In the formula: C _Af -the molar concentration of dye in supercritical carbon dioxide;

C _A0 -the initial dye concentration at the center of the fiber, generally C _A0 =0

The degree of convection coefficient k is affected by the flow state of the dye:

Where: D _Af — the diffusion coefficient of the dye in supercritical carbon dioxide; δ _cf — the thickness of the boundary layer of the dye concentration in supercritical carbon dioxide;

The thickness of the concentration boundary layer δ _cf is also related to the velocity of the flow boundary layer

Where: S _C _{-Schmidt number; ν} -viscosity coefficient of supercritical carbon dioxide; δ ν-thickness of the velocity boundary layer of supercritical carbon dioxide fluid; n-constant;

Where:

—The average velocity of the fluid

ρ—The density of supercritical carbon dioxide dye fluid

η—Viscosity of supercritical carbon dioxide dye fluid

Rex－Reynolds number of dye fluid

Substituting formula (6) into formula (4), we get:

It can be seen from equations (7) and (8) that the greater the fluid velocity, the greater the Rex, and the more severe the convection, the _{smaller the δ cf} , then

The larger the value, the faster the convection on the fiber surface. If the speed of convection is faster than the diffusion speed of the dye from the surface to the inside, the dye will be deposited on the surface, which increases the diffusion resistance of the dye to the inside of the fiber. It is best that the two speeds reach a balance, that is

From the above verification, it can be seen that the use of a pulse syringe to pass the dye solution can increase the pressure P in the dyeing kettle. On the one hand, it increases the saturation concentration of the dye fluid, and enlarges the concentration difference between the dye fluid and the dye in the fiber, and ΔC _A = (C _Af -C _A0 ) will also increase; on the other hand, when the fuel is pulsed, the convection of the dye is strengthened and the mass transfer coefficient is increased. The combination of the two aspects will lead to an increase in the amount of dye deposited on the fiber surface. When the precipitation rate of the dye on the fiber surface is much greater than the diffusion rate inside the fiber, the dye molecules will be deposited on the fiber surface. As the deposition layer thickens, the diffusion resistance of the dye into the fiber is correspondingly increased, and the printing rate is reduced. Therefore, The pressure P must also be reasonably controlled so that the deposition rate of the dye on the fiber surface and the diffusion rate into the fiber are basically balanced.

Application example 2

Based on the pulsed supercritical carbon dioxide printing and dyeing process and device, this application example provides a process for dyeing natural fibers (cotton, linen, and wool fabrics). As shown in Figure 1, the process is composed of seven parts to form a complete automated process, including the CO ₂ storage tank part, the pressurized part, the heating part, the dye mixing part, the auxiliary part, the dual-cycle ultrasonic printing and dyeing part, and the dye cycle section.

When entering the printing and dyeing process, the liquid carbon dioxide _{flows out of the CO 2} storage tank, and sequentially passes through the filter unit, drying unit, heating unit, pressurizing unit, dye tank, auxiliary tank, and feed pump into the dyeing tank through the pulse injector. The yarn spindles preheated and swelled with absolute ethanol and dried are dyed with the dye injected into the dyeing kettle by pulse type under the combined action of KC-TC01 dual-core ultrasonic and two-way circulation pump, and the outer periphery of the dyeing kettle is covered with a thermal insulation layer. At this time, the pressurizing unit (booster pump) needs to pressurize the carbon dioxide pressure to 16MPa; the heating unit (heater) needs to heat the carbon dioxide temperature to 80°C; the supercritical carbon dioxide is separately introduced into the three primary color tanks to dissolve the dye, and then merged The dye liquor is formed in the dye tank; the auxiliary agent tank needs to be added with absolute ethanol as a dye assistant, so that the reactive dye can be more fully dissolved in the supercritical carbon dioxide, so that the dye liquor is more uniform; KC-TC01 dual-core ultrasonic working power is 600W, two-way The circulating pump circulates the dye solution in the dyeing kettle at a speed of 3m/min to improve the uniformity of the dye. The spindle advances and dyes in the dyeing kettle at a rate of 1.2m/min. After the yarn spindle is dyed and matured, it leaves from the spindle end and enters the product collection unit for consignment to the next process. The remaining dye that flows out is not collected by the dye collector, but is directly returned to the dye tank to enter the printing and dyeing cycle for reuse.

Using the above-mentioned application example 1 and application example 2 of the ultra-pulse supercritical carbon dioxide printing and dyeing process and device of the present invention, a spindle can be successfully dyed within 30 minutes, and the spindle will come out from the spindle end at a time interval of about 18 seconds. The length of the equipment can be changed. Control within 30m; Compared with the current process, the efficiency is increased by at least about 20%, the equipment is reduced by about 25%, and the cost is reduced by at least about 10%. The ultra-pulse supercritical carbon dioxide printing and dyeing process and device can realize environmental protection and clean production. , Recycling, high-yield, low-cost use of supercritical carbon dioxide for synthetic fiber and natural fiber printing and dyeing process, and improve the uniformity of the inner and outer fabric dyeing of the spindle, and also improve the color fastness of the fabric, up to 5 level.

The specific embodiments of the present invention are described in detail above, but they are only examples, and the present invention is not limited to the specific embodiments described above. For those skilled in the art, any equivalent modifications and substitutions made to the present utility model are also within the scope of the present utility model. Therefore, the equal transformations and modifications made without departing from the spirit and scope of the present utility model should all be covered within the scope of the present utility model.

Claims

A pulsed supercritical carbon dioxide printing and dyeing device, which is characterized by comprising: a CO 2 storage tank, a three primary color tank, a dye tank, a pulse generator, a dyeing kettle, a dye collection tank, a decompression cooling unit and an extraction separation unit, wherein:

The CO 2 storage tank is connected to the dye tank via the three primary color tanks through the pipeline through the filter unit, the drying unit, the heating unit, and the pressurizing unit in order to pressurize and heat the carbon dioxide in the CO 2 storage tank. Then it is converted into supercritical carbon dioxide, and the supercritical carbon dioxide is mixed with the three primary color dyes in the three primary color tanks in a certain proportion in the dye tank to form a dye solution;

The dye tank is connected to the dyeing tank through a pipeline via an auxiliary tank, a flow meter, and a number of pulse injectors connected in parallel, and each pulse injector is connected to the top and/or bottom of each section of the dyeing tank in turn. A number of liquid inlet holes are arranged, which are used to send the dye solution into each section of the dyeing kettle by pulse injection through the pulse injector to dye the spindles from the end of the spindle; each section of the dyeing kettle A dual-core ultrasonic generating device and a two-way circulation pump are provided on the two-way circulation pump. Both ends of the two-way circulation pump are connected to the pulse syringe and the dyeing kettle with Y-shaped connectors, and the two Y-shaped connectors are located in each section. The liquid inlet holes at both ends of the bottom of the dyeing kettle;

The bottom of the dyeing tank is connected to the dye tank through a pipe to return the remaining dye liquor discharged from the dyeing tank to the dye tank for recycling; or the bottom of the dyeing tank is connected to the dye collection tank through a pipe to remove The remaining dye liquor after dyeing in the dyeing kettle is collected in the dye collection tank, and after separation and purification is processed into liquid carbon dioxide and dyes, it is transported as liquid carbon dioxide raw materials and dye raw materials to the CO 2 storage tank and dyes respectively through pipelines. The tank is recycled or stored for later use.
The pulsed supercritical carbon dioxide printing and dyeing device according to claim 1, wherein the bottom of the dyeing kettle is connected to the decompression cooling unit through the dye collection tank through a pipe, so as to dye the inside of the dyeing kettle. The remaining dye liquor is collected in the dye collection tank, and the remaining dye liquor is decompressed and separated through the decompression cooling unit.
The pulsed supercritical carbon dioxide printing and dyeing device according to claim 1, wherein the top of the decompression cooling unit is connected to the CO 2 storage tank through a pipeline through a purification unit, a filter unit and a drying unit to separate the CO 2 storage tank. The latter carbon dioxide gas is sent to the CO 2 storage tank for recycling.
The pulsed supercritical carbon dioxide printing and dyeing device according to claim 1, wherein the bottom end of the decompression cooling unit is connected to the extraction separation unit through a pipe, so that the separated dye liquor is subjected to extraction treatment, and the extracted dye The dye tank is sent to the dye tank for recycling, and/or the extracted auxiliary is sent to the auxiliary tank for recycling.
The pulsed supercritical carbon dioxide printing and dyeing device according to claim 1, wherein the dyeing kettle is composed of a pipe of 24-25 meters and covered with a thermal insulation layer.
The pulsed supercritical carbon dioxide printing and dyeing device according to claim 1, wherein the dyeing kettle is divided into four sections along its length, and each section of the dyeing kettle is provided with the pulse injector and the ultrasonic generator. And two-way circulation pump.
The pulsed supercritical carbon dioxide printing and dyeing device according to claim 6, characterized in that, liquid inlet holes are respectively opened at 1000mm, 3000mm, and 5000mm from the outlet end of each section of the dyeing kettle, and the liquid inlet holes pass A pipe is connected to the pulse injector.
The pulsed supercritical carbon dioxide printing and dyeing device according to claim 6, characterized in that, liquid drainage holes are respectively opened at 375mm, 625mm, 875mm, and 1125mm from the outlet end of each section of the dyeing kettle, and the drainage The hole connects the dye tank and the dye collection tank through a pipe.
The pulsed supercritical carbon dioxide printing and dyeing device according to claim 8, wherein the liquid discharge hole and the liquid inlet hole both have a small and small head structure, and both are composed of an upper hole and a lower hole.
The pulsed supercritical carbon dioxide printing and dyeing device according to claim 1, wherein the axis angle between the two ports in the double port direction on the Y-shaped port is 90°.