Supercritical carbon dioxide waterless dyeing kettle, dyeing system and dyeing method

By setting a spiral flow guiding structure in the jacket of the supercritical anhydrous dyeing vessel, the problem of uneven heat caused by the single flow path of the heat transfer medium is solved, thereby improving the temperature uniformity and heat exchange efficiency in the dyeing chamber.

CN121023768APending Publication Date: 2025-11-28FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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Patent Information

Application Number
CN202511202215.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-08-26
Publication Date
2025-11-28

AI Technical Summary

Technical Problem

The existing supercritical anhydrous dyeing kettle has a single flow path for the heat transfer medium, resulting in uneven heat distribution and a significant temperature gradient within the dyeing chamber, which affects dyeing uniformity and fiber stability.

Method used

A spiral flow guide structure is installed inside the heating and cooling jacket device to extend the flow path of the heat transfer medium. The medium is guided to flow spirally along the outer wall of the dyeing vessel through the spiral guide plate, thereby enhancing the uniformity of heat distribution.

Benefits of technology

It significantly improves the temperature uniformity within the dyeing chamber, avoids color spots and fiber melting problems caused by local overheating and excessive temperature differences, and enhances heat exchange efficiency.

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Abstract

The invention discloses a supercritical waterless dyeing kettle, a dyeing system and a dyeing method.The dyeing kettle at least comprises a dyeing kettle body, the dyeing kettle body comprises a closed end and an open end, and a dyeing cavity is formed in the dyeing kettle body; the kettle cover is fixedly connected with the open end of the dyeing kettle body and closes the open end; the heating and cooling jacket device is fixed outside the dyeing kettle body in a sleeving manner, the heating and cooling jacket device is of a hollow structure, and a medium with a heating or cooling function is introduced into the heating and cooling jacket device; the dyeing warp beam is arranged in the middle of a dyeing cavity of the dyeing kettle body, the dyeing warp beam is a hollow pipe body, and a plurality of fluid permeation holes are formed in the pipe wall of the dyeing warp beam; wherein a spiral flow guide structure is further arranged in the heating and cooling jacket device, and the spiral flow guide structure is arranged along the outer wall of the dyeing kettle body. The method is suitable for implementing efficient and uniform waterless dyeing treatment on the textile by using the supercritical carbon dioxide medium.
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Description

Technical Field

[0001] This invention relates to the technical field of supercritical fluid dyeing equipment, specifically to a supercritical carbon dioxide anhydrous dyeing kettle, system, and method of use. More particularly, it relates to a supercritical carbon dioxide anhydrous dyeing kettle with a spiral guide plate inside the jacket and its application, suitable for efficient and uniform anhydrous dyeing of textiles using supercritical carbon dioxide media. Background Technology

[0002] Traditional textile dyeing processes in my country primarily use water as the dyeing medium, relying on water to carry dyes and color the textiles. In actual production, this type of process not only requires large amounts of water for washing, bleaching, and dyeing, but also necessitates the addition of significant amounts of auxiliaries, dispersants, and stabilizers at each stage. This results in a high water consumption, high energy consumption, and high pollution rate, placing a severe burden on the environment, particularly in wastewater treatment. Therefore, developing green, clean, and efficient dyeing technologies to reduce environmental pollution and resource consumption has become a development trend in the textile dyeing and finishing industry.

[0003] Supercritical carbon dioxide anhydrous dyeing technology, as an emerging green dyeing method, is considered an important alternative to traditional water-based dyeing processes. This technology uses supercritical carbon dioxide fluid instead of water as the dyeing medium. Under high temperature and pressure, the dye is dissolved in supercritical carbon dioxide and then enters the dyeing kettle along with the fluid, ensuring full contact with the fabric and achieving dye uptake. After dyeing, the supercritical carbon dioxide is converted to a gaseous state by reducing the system pressure, achieving medium separation and recovery. Unused dye is recovered in solid form, and the entire process generates virtually no wastewater. Compared to traditional dyeing and finishing processes, this process generally requires only one dyeing step, simultaneously completing multiple processes such as dyeing, reduction, washing, and drying, significantly shortening the production cycle and improving production efficiency. Furthermore, this process requires no auxiliaries or chemical solvents, is clean, and generates no waste liquid, effectively alleviating the high water consumption and high pollution problems in the textile printing and dyeing industry, possessing significant environmental advantages and promising industrialization prospects.

[0004] Supercritical carbon dioxide anhydrous dyeing processes require high-temperature environments. Currently, jacketed heating structures are commonly used to heat the dyeing vessel, where a jacket is installed on the outer wall of the vessel, and a circulating heat transfer medium is used to heat and maintain the dyeing chamber. However, the flow channel design of traditional jacketed devices is usually quite simple, and the heat transfer medium tends to flow along the shortest path from the inlet to the outlet, causing a "short-circuit effect." This effect leads to uneven heat distribution within the jacket, resulting in a significant temperature gradient in the dyeing chamber. When the local temperature is too high, it can easily induce thermal sublimation or deposition of disperse dyes, forming color spots on the fabric surface, and even causing thermal damage such as melting and cracking of heat-sensitive fibers (see...).Figure 3 This seriously affects the uniformity and stability of dyed products.

[0005] Therefore, optimizing the internal structure of the jacket, rationally guiding the flow path of the heat transfer medium within the jacket, avoiding heat accumulation in local areas, and improving heat exchange efficiency and the uniformity of the temperature field in the dyeing chamber are key issues that urgently need to be addressed in current supercritical anhydrous dyeing equipment technology. Summary of the Invention

[0006] To address the technical problems existing in current supercritical anhydrous dyeing kettles, such as the single flow path of the heat-conducting medium, uneven heat distribution, and significant temperature gradients within the dyeing chamber, this invention provides a supercritical carbon dioxide anhydrous dyeing kettle, dyeing system, and dyeing method. This significantly extends the flow path of the heat-conducting medium within the jacket, improves its flow distribution and disturbance intensity, and makes the heat distribution on the outer wall of the kettle more uniform, thereby effectively improving the temperature uniformity within the dyeing chamber.

[0007] To achieve the above objectives, the present invention provides the following technical solution:

[0008] A supercritical anhydrous staining vessel, the staining vessel comprising at least:

[0009] A dyeing vessel body, comprising a closed end and an open end, wherein a dyeing chamber is provided inside the dyeing vessel body;

[0010] A lid is fixedly connected to the open end of the dyeing vessel body and closes the open end.

[0011] A heating and cooling jacket device is fitted and fixed to the outside of the dyeing vessel body. The heating and cooling jacket device has a hollow structure and is filled with a medium that has heating or cooling functions.

[0012] A dyeing warp shaft is located in the middle of the dyeing chamber of the dyeing vessel. The dyeing warp shaft is a hollow tube with multiple fluid permeation holes on its tube wall.

[0013] The heating and cooling jacket device is also equipped with a spiral flow guiding structure, which is arranged along the outer wall of the dyeing vessel.

[0014] In an alternative embodiment of the present invention, a multi-layer cylindrical structure is provided between the jacket of the heating and cooling jacket device and the dyeing vessel body.

[0015] In an alternative embodiment of the present invention, the spiral guide structure is a spiral guide plate, which is arranged in a spiral shape and welded and fixed to the outer wall of the dyeing vessel in a spiral-encircling manner.

[0016] In an alternative embodiment of the present invention, the thickness of the baffle of the spiral guide plate is 2-10 mm, the pitch is 100-500 mm, and the number of spiral turns is 5-10.

[0017] In an alternative embodiment of the invention, the spiral guide plate is made of stainless steel S30408.

[0018] In an alternative embodiment of the present invention, the heating and cooling jacket device is further provided with a heat transfer medium inlet and a heat transfer medium outlet. The heat transfer medium inlet is arranged at one end of the heating and cooling jacket device near the vessel lid, and the heat transfer medium outlet is arranged on the other side of the heating and cooling jacket device. The heat transfer medium inlet and the heat transfer medium outlet are located on the same side of the heating and cooling jacket device and communicate with the internal space of the heating and cooling jacket device.

[0019] In an alternative embodiment of the present invention, the dyeing vessel body is further provided with a carbon dioxide outlet and a carbon dioxide inlet, the carbon dioxide outlet and the carbon dioxide inlet being connected to the dyeing chamber respectively. The carbon dioxide outlet is located on the outer wall of the dyeing vessel body near the open end and extends outward through the heating and cooling jacket device to form an interface. The carbon dioxide inlet is located at the closed end of the dyeing vessel body, connected to one end of the dyeing warp shaft, and extends outward through the heating and cooling jacket device to form an interface.

[0020] In an alternative embodiment of the present invention, the dyeing vessel body is arranged horizontally, and the dyeing warp shaft is fixedly placed in the dyeing vessel body in a horizontal manner.

[0021] In an alternative embodiment of the present invention, the dyeing vessel is provided with three carbon dioxide outlets, which are evenly spaced along the circumferential direction, and the three carbon dioxide outlets are collected by a flow collection structure and then connected to a pipe for recycling and outflow.

[0022] In an alternative embodiment of the present invention, circular sealing baffles are fixed at both ends of the dyeing warp shaft, and a temperature measuring device for measuring the temperature distribution data of the outer wall of the dyeing vessel is also provided on the outer wall surface of the dyeing vessel body. The temperature measuring device includes multiple patch-type temperature sensors arranged along the axial direction of the dyeing vessel body, and a set of temperature measuring points are respectively set in the upper, middle and lower regions of the vessel body.

[0023] In an alternative embodiment of the present invention, the diameter of the circular sealing baffle is 460 mm, the thickness is 20 mm, and the axial distance between the two circular sealing baffles is 1800 mm.

[0024] In an alternative embodiment of the present invention, the temperature sensor is connected to a thermocouple digital thermometer to acquire temperature distribution data of the outer wall of the dyeing vessel in real time.

[0025] In an alternative embodiment of the present invention, both the inlet and outlet ends of the heat transfer medium are provided with connecting flanges, and the rear end of the connecting flanges is connected to a heat transfer oil pipe with an outer diameter of 32 mm and a wall thickness of 3.5 mm.

[0026] In an alternative embodiment of the present invention, the fluid permeation holes are evenly distributed on the outer wall of the dyeing warp shaft, with a total of 15 rows arranged along the axial direction of the dyeing warp shaft. Each row is arranged at a circumferential angle interval of 24°, and each row has 72 holes with a hole spacing of 25 mm and a hole diameter of 10 mm.

[0027] The present invention also provides a supercritical carbon dioxide anhydrous dyeing system, the dyeing system comprising the above-mentioned supercritical anhydrous dyeing kettle, and a carbon dioxide pressurization supply device, a color matching device, a circulation device and a separation and recovery device, all connected to the supercritical anhydrous dyeing kettle and controlled by an automatic control system;

[0028] The staining system includes two supercritical anhydrous staining vessels, which are arranged in parallel. The pressurization time of the second supercritical anhydrous staining vessel is reduced by equalizing the pressure.

[0029] In an alternative embodiment of the present invention, the color mixing device includes a color mixing vessel and a dye box disposed inside the color mixing vessel; the outlet of the color mixing vessel is connected to the carbon dioxide inlet of the supercritical anhydrous dyeing vessel.

[0030] In an alternative embodiment of the invention, the color mixing vessel is arranged vertically.

[0031] In an alternative embodiment of the invention, the dye cartridge is provided with a guide impeller and a vortex booster.

[0032] In an alternative embodiment of the invention, the circulation device includes a circulation pump and a heat exchanger, and the supercritical anhydrous dyeing vessel is connected to the circulation pump and the heat exchanger respectively via circulation pipes.

[0033] In an alternative embodiment of the present invention, the inner wall of the color mixing vessel, the inner wall of the dyeing vessel body, and the inner wall of the circulating pipe connected thereto are all provided with a non-stick coating.

[0034] In an alternative embodiment of the invention, the operating temperature of the circulation device is 80-150°C and the operating pressure is 23-35 MPa.

[0035] In an alternative embodiment of the invention, the operating temperature of the circulation device is 110°C and the operating pressure is 23 MPa.

[0036] In an alternative embodiment of the present invention, the separation and recovery device includes a high-pressure recovery component and a low-pressure recovery component; the high-pressure recovery component includes a condenser, a separation vessel, and a filter in sequence; the low-pressure recovery component includes a low-pressure compressor, a tail gas storage tank, and a filter in sequence; the carbon dioxide outlet of the supercritical anhydrous dyeing vessel is connected to the condenser and the low-pressure compressor, respectively.

[0037] In an alternative embodiment of the present invention, both the separation vessel and the filter are two-stage designs, with a primary separation vessel and a secondary separation vessel, as well as a primary filter and a secondary filter.

[0038] In an alternative embodiment of the present invention, carbon dioxide passes through a carbon dioxide storage tank, a pressurizing pump and a preheater, and then enters the color mixing kettle through a circulation pipe. The outlet of the color mixing kettle is connected to the carbon dioxide inlet of the supercritical anhydrous dyeing kettle. The supercritical anhydrous dyeing kettle is connected to the circulation pump and the heat exchanger through circulation pipes to form a dyeing circulation mechanism.

[0039] The carbon dioxide circulation outlet of the supercritical anhydrous dyeing kettle is connected to the condenser to cool and depressurize the dye liquor after dyeing. Then, the carbon dioxide and dye are separated by a multi-stage separation kettle. Finally, the carbon dioxide is pumped into the carbon dioxide storage tank by a transfer pump.

[0040] The present invention also provides a staining method for a supercritical carbon dioxide anhydrous staining system, the staining method comprising:

[0041] The dyeing warp beam with the fabric to be dyed wound around it is placed in the supercritical anhydrous dyeing kettle mentioned above, and the dye is placed into the color matching device.

[0042] Carbon dioxide gas is introduced into the staining system, and the system is heated and pressurized to the set parameters;

[0043] After the temperature and pressure in the dyeing system stabilize to the preset value, the circulation device is turned on to perform dyeing cycle until the specified dyeing time is reached.

[0044] After dyeing is completed, the separation and recovery device is activated to recover the residual carbon dioxide medium in the system.

[0045] In an alternative embodiment of the invention, the dyeing method further includes measuring the temperature of the outer wall of the dyeing vessel using a thermocouple digital thermometer during the dyeing cycle.

[0046] The beneficial effects of this invention are:

[0047] This invention significantly extends the flow path of the heat-conducting medium in the jacket, making it evenly distributed on the outer wall of the dyeing chamber, enhancing its contact and convection with the heat exchange surface, thereby reducing the maximum temperature difference on the outer wall of the dyeing vessel from 13°C to 3°C, avoiding thermal damage problems such as color spots and fiber melting caused by local overheating or excessive temperature difference. Attached Figure Description

[0048] Figure 1 This is a schematic diagram of the structure of an existing dyeing vessel;

[0049] Figure 2 This is a schematic diagram of the structure of the supercritical anhydrous dyeing vessel of the present invention;

[0050] Figure 3 These are photos of actual products showing color spots and nonwoven fabric meltdown caused by uneven temperature during the dyeing process.

[0051] Figure 4 A schematic diagram of a model of an existing dyeing vessel used for simulation calculations and the dyeing vessel of the present invention;

[0052] Figure 5 A comparison diagram of the streamline distribution of the heat-conducting medium in existing dyeing kettles and the dyeing kettle of the present invention;

[0053] Figure 6 A comparison diagram of the temperature field distribution inside the dyeing chamber of an existing dyeing vessel and the dyeing vessel of the present invention;

[0054] Figure 7 This is a schematic diagram of the supercritical anhydrous staining system equipment of Embodiment 2 of the present invention.

[0055] Reference numerals: 1-Dyeing chamber, 2-Dyeing vessel body, 3-Temperature measuring device, 4-Vessel cover, 5-Heating and cooling jacket device, 6-Fluid permeation hole, 7-Dyeing warp shaft, 8-Baffle, 9-Heat transfer medium inlet, 10-Heat transfer medium outlet, 11-Connecting flange, 12-Carbon dioxide outlet, 13-Carbon dioxide inlet, 14-Spiral guide plate, 15-Carbon dioxide storage tank, 16-Pressure pump, 17-Preheater, 18-Color matching vessel, 19-Dyeing vessel, 20-Circulation pump, 21-Heat exchanger, 22-Condenser, 23-Multi-stage separation vessel, 24-Transfer pump. Detailed Implementation

[0056] To make the objectives, technical solutions, and advantages of this application clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0057] Embodiments of the present invention, examples of which are shown in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The terms "first," "second," "third," etc., in the specification, claims, and drawings of the present invention (if present) are used to distinguish similar objects and are not necessarily used to describe a specific order or sequence. It should be understood that such described objects can be interchanged where appropriate. Furthermore, the terms "comprising" and "having," and any variations thereof, are intended to cover non-exclusive inclusion. Directional terms used in the present invention, such as: up, down, left, right, front, back, inside, outside, side, etc., are only for the purpose of referring to the drawings. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain the present invention, and should not be construed as limiting the present invention. Furthermore, the present invention repeats reference numerals and / or reference letters in different examples; this repetition is for simplification and clarity and does not in itself indicate a relationship between the various embodiments and / or arrangements discussed. In addition, the present invention provides examples of various specific processes and materials, but those skilled in the art will recognize the application of other processes and / or the use of other materials.

[0058] Example 1

[0059] like Figure 2 As shown, the supercritical anhydrous dyeing vessel of this embodiment includes at least: a dyeing vessel body 2, a vessel cover 4, a heating and cooling jacket device 5, a dyeing warp shaft 7, and a spiral guide plate 14.

[0060] The dyeing kettle body 2 includes a closed end and an open end, and a dyeing chamber 1 is provided inside the dyeing kettle body 2. Specifically, the dyeing kettle body 2 is arranged horizontally. The dyeing chamber 1 is used to accommodate textiles for dyeing treatment.

[0061] Furthermore, the dyeing vessel body 2 is also provided with a carbon dioxide outlet 12 and a carbon dioxide inlet 13, which are respectively connected to the dyeing chamber 1. The carbon dioxide outlet 12 enables the dyeing chamber 1 to communicate with the outside world and release gas.

[0062] Carbon dioxide outlet 12 is located on the outer wall of the dyeing vessel 2 near the open end, and extends outward through the heating and cooling jacket device 5 to form an interface. Carbon dioxide inlet 13 is located at the closed end of the dyeing vessel 2, communicates with one end of the dyeing shaft 7, and extends outward through the heating and cooling jacket device 5 to form an interface, connecting to the media supply end and recovery end of the dyeing system respectively.

[0063] Preferably, the dyeing vessel body 2 is provided with three carbon dioxide outlets 12, which are evenly spaced at 120° angles along the circumference. The three carbon dioxide outlets 12 are collected by a flow collection structure and then connected to a single pipe for recycling.

[0064] A temperature measuring device 3 for measuring the temperature distribution data of the outer wall of the dyeing vessel 2 is also provided on the outer wall surface of the dyeing vessel 2. The temperature measuring device 3 is fixedly installed on the outer wall of the dyeing vessel 2. The temperature measuring device 3 can be a patch thermocouple temperature measuring device. Preferably, the temperature measuring device 3 includes multiple patch temperature sensors, which can be connected to a thermocouple digital thermometer to acquire the temperature distribution data of the outer wall of the dyeing vessel 2 in real time. Preferably, the multiple patch temperature sensors are arranged along the axial direction of the dyeing vessel 2, and a set of temperature measuring points is set in the upper, middle, and lower regions of the dyeing vessel 2.

[0065] The lid 4 is fixedly connected to the open end of the dyeing vessel body 2 and closes the open end. The lid 4 is placed on the dyeing vessel body 2 to open and close the opening of the dyeing chamber 1.

[0066] Furthermore, clamps are provided on the outside of the kettle lid 4 and the dyeing kettle body 2 to lock and seal the dyeing kettle. These clamps are quick-opening clamp types.

[0067] Preferably, the outer side of the dyeing vessel body 2 is provided with a moving drive device for driving the vessel lid 4 to move longitudinally to open and close the opening of the dyeing chamber 1. After the vessel lid 4 is closed, the clamp can be quickly opened and closed through mechanical control. Optionally, the moving drive device can also be any other existing device capable of driving the vessel lid 4 to move.

[0068] The heating and cooling jacket device 5 is used to heat the dyeing vessel body 2. It is sleeved and fixed to the outside of the dyeing vessel body 2, surrounding the outer wall of the dyeing vessel body 2, and sealed to the outer wall of the dyeing vessel body 2. The heating and cooling jacket device 5 has a hollow structure, and a medium with heating or cooling function is introduced into it. This medium is a substance capable of heat exchange, such as water, oil, or gas. Preferably, the medium is heat transfer oil.

[0069] Preferably, a multi-layer cylindrical structure is provided between the heating and cooling jacket device 5 and the dyeing kettle body 2 to enhance the structural stability of the entire dyeing kettle equipment.

[0070] Furthermore, the heating and cooling jacket device 5 is also provided with a heat transfer medium inlet 9 and a heat transfer medium outlet 10. The heat transfer medium inlet 9 is arranged at one end of the heating and cooling jacket device 5 near the vessel cover 4, and the heat transfer medium outlet 10 is arranged on the other side of the heating and cooling jacket device 5. The heat transfer medium inlet 9 and the heat transfer medium outlet 10 are located on the same side of the heating and cooling jacket device 5 and are connected to the internal space of the heating and cooling jacket device 5 to form a closed-loop heat exchange path.

[0071] Furthermore, both the inlet 9 and outlet 10 of the heat transfer medium are provided with connecting flanges 11 for sealing connection, used to connect the heat transfer medium pipeline. The outer diameter of the heat transfer medium pipeline is 30-600mm, and the wall thickness is 3.5-10mm. Preferably, the rear end of the connecting flange 11 can be connected to a heat transfer medium pipeline with an outer diameter of 32mm and a wall thickness of 3.5mm.

[0072] Preferably, since the dyeing vessel body 2 is arranged horizontally, the heat transfer medium inlet 9 and the heat transfer medium outlet 10 are located on the upper side of the heating and cooling jacket device 5, and the flow pattern is top-in and top-out.

[0073] The heating and cooling jacket device 5 is also equipped with a spiral flow guiding structure. The spiral flow guiding structure is set along the outer wall of the dyeing kettle body 2 to guide the medium introduced into the heating and cooling jacket device 5 to flow along the spiral path of the outer wall.

[0074] Specifically, the spiral guide structure is a spiral guide plate 14, which is arranged in a spiral shape and is welded and fixed to the outer wall of the dyeing vessel body 2 in a spiral winding manner.

[0075] Optionally, the thickness of the baffle of the spiral guide plate 14 is 2-10 mm, the pitch is 100-500 mm, and the number of spiral turns is 5-10. Preferably, the thickness of the baffle of the spiral guide plate 14 is 2 mm, the pitch is 250 mm, the number of spiral turns is 7, and it is arranged around the outer wall of the dyeing vessel body 2 in a clockwise direction.

[0076] Optionally, the spiral guide plate 14 is made of stainless steel S30408 ​​to adapt to long-term stable operation under high temperature and high pressure environment, with good corrosion resistance and high mechanical strength, and is not easy to crack or deform during the flow guiding process.

[0077] The dyeing warp spindle 7 is located in the middle of the dyeing chamber 1 of the dyeing vessel body 2. It is used to support, hold, and wind the fabric to be dyed. The dyeing warp spindle 7 is a hollow tube with multiple fluid permeation holes 6 on its wall. The dyeing warp spindle 7 is horizontally fixed inside the dyeing vessel body 2. The diameter of the fluid permeation holes 6 is 4-10 mm, and the hole spacing is 5-25 mm.

[0078] Furthermore, the fluid permeation holes 6 are evenly distributed on the outer wall of the dyeing warp shaft 7. Preferably, the fluid permeation holes 6 are arranged in 15 rows along the axial direction of the dyeing warp shaft 7, with each row spaced at a circumferential angle of 24°. Each row has 72 holes with a hole spacing of 25 mm and a hole diameter of 10 mm.

[0079] One end of the dyeing shaft 7 is connected to the carbon dioxide inlet 13, and the other end is the exhaust or closed end.

[0080] Furthermore, circular sealing baffles 8 are fixed at both ends of the dyeing warp shaft 7.

[0081] Optionally, the diameter of the circular sealing baffle 8 is 460 mm and the thickness is 20 mm. The axial distance between the two circular sealing baffles 8 is 800-3000 mm, preferably 1800 mm.

[0082] Furthermore, the working volume of the dyeing vessel 2 is 20-10000L, the working pressure is 20-35MPa, and the working temperature is 80-150℃. The working volume of the matching heating and cooling jacket device 5 is 1-1000L, the working pressure is 0.3-0.6MPa, and the working temperature is 80-150℃.

[0083] Preferably, the working volume of the dyeing vessel 2 is 450L, the working pressure is 20-25MPa, and the working temperature is 90-110℃.

[0084] Preferably, the heating and cooling jacket device 5 has a working volume of 350L, a working temperature of 90-110℃, and a working pressure of 23Mpa.

[0085] Furthermore, all exposed heat-conducting medium pipes and the outer wall of the dyeing vessel 2 are covered with insulating cotton material to reduce heat loss. Preferably, the outer side of the heating and cooling jacket device 5 is covered with silicate insulating cotton.

[0086] To further verify the effectiveness of the spiral flow guiding structure proposed in this embodiment in optimizing the flow path of the heat transfer medium and improving the temperature uniformity of the staining cavity, a non-spiral flow guiding structure (such as...) was used. Figure 1 (as shown) and dyeing kettles equipped with spiral flow guiding structures (such as...) Figure 2 The two structures (shown in the figure) are used as the research objects, and the Fluent fluid simulation software is used to conduct flow heat transfer simulation analysis.

[0087] The thermal field simulation verification method includes the following steps:

[0088] Three-dimensional finite element simulation models were established for two types of supercritical anhydrous dyeing kettles, one with a spiral flow guiding structure and the other without. Fluent software was used to simulate the flow heat transfer. By comparing and analyzing the streamline diagram of the heat-conducting medium in the jacket and the temperature distribution cloud diagram of the dyeing cavity, the effect of the spiral flow guiding structure on improving the heat conduction path and temperature field uniformity was verified.

[0089] Preferably, the simulation results are verified by actual dyeing and temperature measurement experiments under the same operating conditions as the calculation settings.

[0090] Specifically, such as Figure 4As shown, two computational models of supercritical carbon dioxide anhydrous dyeing reactors were established: one with a spiral flow guiding structure and the other without. This supercritical anhydrous dyeing reactor computational model comprises three regions: a heat-conducting medium fluid domain, a dyeing chamber fluid domain, and a solid-state heat transfer domain between the two.

[0091] To ensure simulation accuracy and consistency between the two models, both simulation models used the same meshing parameters. The minimum mesh size was set to 1 mm, and the maximum size to 5 mm, using a poly-hexahedral core hybrid meshing strategy. The resulting mesh contains approximately 14 million elements, with a maximum skewness of 0.56 and a minimum orthogonal mass of 0.2, all meeting Fluent's minimum mesh quality requirements for turbulent heat transfer problems.

[0092] Import the generated mesh into Fluent software and perform calculations in steady-state solution mode. First, enable the gravity effect and set the gravitational acceleration to 9.81 m / s². 2 To take into account the influence of gravity on the natural convection and flow distribution of the heat-conducting medium.

[0093] In terms of physical model setup, the standard k-epsilon turbulence model was selected in conjunction with the enhanced wall treatment method, and the energy equation was enabled to solve the heat transfer process between the heat-conducting medium, the solid wall, and the fluid in the cavity.

[0094] The heat transfer medium is industrial-grade heat transfer oil, and its physical properties such as density, viscosity, specific heat capacity, and thermal conductivity are added by customization. The fluid domain of the staining chamber is supercritical carbon dioxide, and its physical properties are called from the Fluent's built-in NIST database. All components in the solid domain are made of stainless steel, and their physical properties are called and set through the "steel" item in the Fluent's built-in material library.

[0095] The boundary conditions are set as follows: both the heat transfer oil and the supercritical carbon dioxide inlet adopt constant mass flow boundary conditions, with the heat transfer oil mass flow rate set to 10 kg / s and the inlet temperature to 130℃; the supercritical carbon dioxide mass flow rate is set to 12.5 kg / s and the inlet temperature to 110℃. The outer wall of the dyeing vessel is set as an adiabatic boundary condition to avoid external heat loss from the system; the partition between the heat transfer oil and the supercritical carbon dioxide adopts a wall-coupled heat exchange setting to achieve effective heat transfer from the high-temperature heat transfer oil through the stainless steel wall to the supercritical carbon dioxide fluid in the dyeing chamber.

[0096] The numerical solution method adopts the SIMPLE first-order scheme algorithm to ensure the convergence of steady-state calculation.

[0097] After the calculation results converged, the streamline diagram of the heat transfer oil in the jacket and the steady-state temperature distribution cloud map of the supercritical carbon dioxide in the dyeing chamber were plotted respectively.

[0098] Figure 5 The diagram shows a comparison of the flow paths of the heat transfer oil under two different structures. As can be seen from the figure, in the model without the spiral guide plate, the heat transfer oil mainly flows parabolically along the shortest path between the inlet and outlet. A significant "short-circuit effect" exists inside the jacket, with localized areas experiencing low flow velocities or even stagnation, resulting in low utilization of the heat exchange surface and limited heat exchange efficiency. In the structure proposed in this embodiment, the spiral guide plate effectively guides the heat transfer oil to form a spiral path along the outer wall of the vessel, resulting in a more uniform flow trajectory, a significantly extended heat exchange path, enhanced fluid turbulence, and a substantial increase in the coverage area of ​​the heat transfer oil on the heat exchange surface, thereby achieving a more complete heat transfer process.

[0099] Figure 6 The temperature distribution contour maps of supercritical carbon dioxide within the staining chamber under two different structures are presented. Simulation results show that without the spiral guide structure, the temperature field distribution inside the staining chamber is significantly uneven, with localized overheating and a significant temperature gradient. However, after introducing the spiral guide plate, the uniformity of the temperature distribution within the staining chamber is significantly improved, effectively suppressing the formation of localized overheating and large temperature difference regions.

[0100] Therefore, the simulation results verify the significant effects of the spiral flow guiding structure proposed in this embodiment in optimizing the heat transfer path of the heat transfer medium, improving heat exchange efficiency, enhancing heat conduction uniformity, and improving temperature field distribution.

[0101] Example 2

[0102] This embodiment provides a supercritical carbon dioxide anhydrous dyeing system. The dyeing system includes the supercritical anhydrous dyeing kettle described in the above embodiment, as well as a carbon dioxide pressurization supply device, a color matching device, a circulation device, and a separation and recovery device, all connected to the supercritical anhydrous dyeing kettle and controlled by an automatic control system.

[0103] The carbon dioxide pressurization supply device includes a carbon dioxide storage tank 15, a pressurization pump 16, and a preheater 17. The pressurization pump 16 is responsible for filling the circulation pipeline with carbon dioxide, so that the fluid pressure in the pipeline reaches the process pressure; the function of the preheater 17 is to heat the fluid to the preset temperature, saving the heating time required in the subsequent dyeing process.

[0104] Preferably, the staining system includes two supercritical anhydrous staining vessels, which are arranged in parallel, and the pressurization time of the second supercritical anhydrous staining vessel is reduced by equalizing the pressure.

[0105] The color mixing device includes a color mixing vessel 18 and a dye box disposed inside the color mixing vessel 18. The outlet of the color mixing vessel 18 is connected to the carbon dioxide inlet 13 of the supercritical anhydrous dyeing vessel 19. The dye box is equipped with a guide impeller and a vortex aid to enhance the dissolution of the dye.

[0106] Optionally, the color mixing vessel can be arranged vertically.

[0107] The circulation device includes at least one circulation pump 20 and at least one heat exchanger 21. The supercritical anhydrous dyeing vessel is connected to the circulation pump 20 and the heat exchanger 21 respectively through circulation pipes, forming a dyeing circulation mechanism. Among them, the heat exchanger 21 is used for the condensation and liquefaction of carbon dioxide during the dyeing circulation process, heating the liquid carbon dioxide to the supercritical state to supplement the heat required for the isothermal desorption process of throttling and depressurization.

[0108] Furthermore, the inner wall of the color mixing vessel 18, the inner wall of the dyeing vessel body 2 of the dyeing vessel 19, and the inner wall of the circulating pipe connected to them are all provided with a non-stick coating.

[0109] The operating temperature of the circulation device is 80-150℃, and the operating pressure is 23-35MPa. Preferably, the operating temperature of the circulation device is 110℃, and the operating pressure is 23MPa.

[0110] The separation and recovery device includes a condenser 22, a multi-stage separation vessel 23, and a transfer pump 24. The pipeline formed by the carbon dioxide circulation outlet of the supercritical anhydrous dyeing vessel is connected to the condenser 22 to cool and depressurize the dye liquor after dyeing, so that the carbon dioxide is restored from the supercritical state to the gaseous state. Then, the carbon dioxide and dye are separated by the multi-stage separation vessel 23, and finally the carbon dioxide is introduced into the carbon dioxide storage tank 15 by the transfer pump 24.

[0111] Preferably, the multi-stage separation vessel is a two-stage design, including a primary separation vessel and a secondary separation vessel.

[0112] Example 3

[0113] This embodiment provides a staining method applied to the supercritical carbon dioxide anhydrous staining system described in the above embodiments. This staining method can also verify the reliability of simulation results. The staining method includes:

[0114] S100. The dyeing warp 7, on which the fabric to be dyed is wound, is placed inside the dyeing vessel body 2 of the supercritical anhydrous dyeing vessel of the above embodiment, and the dye is placed into the color matching vessel of the color matching device, wherein the dye is obtained by weighing.

[0115] Specifically, first, open the kettle lid 4, push the dyeing warp beam 7 with the fabric to be dyed wrapped around it into the dyeing kettle body 2, weigh a certain amount of dye and put it into the color mixing kettle 18, and close the kettle lid 4 and seal the color mixing kettle 18 through the automatic control system.

[0116] S200. Carbon dioxide gas is introduced into the dyeing system, and the system is heated and pressurized to the set process parameters. The process parameters are consistent with the boundary conditions used in the simulation calculations of Example 1.

[0117] Specifically, the carbon dioxide pressurization supply device is then started. The carbon dioxide enters the circulation pipeline through the pressurization pump 16, is heated in the preheater 17, and then pressurized by the pressurization pump, and is then introduced into the color mixing tank 18 and the dyeing tank 19 respectively.

[0118] S300. After the temperature and pressure in the dyeing system stabilize to the preset value, start the circulation pump 20 of the circulation device to perform dyeing circulation until the specified dyeing time is reached.

[0119] Specifically, when the internal temperature of the dyeing vessel 19 reaches 110°C and the pressure reaches 23MPa, the circulation pump 20 is turned on to perform dyeing circulation.

[0120] During the dyeing cycle, supercritical carbon dioxide fluid enters the color mixing tank 18 to dissolve the dye, and then carries the dye solution into the dyeing tank 19 for continuous dyeing of the fabric to be dyed. During this stage, the dye is continuously dissolved and circulated, while the temperature distribution data of each temperature measuring point on the outer wall of the dyeing tank is monitored and recorded in real time using the temperature measuring device 3.

[0121] S400 After dyeing is completed, start the separation and recovery device to recover the residual carbon dioxide medium in the system.

[0122] Specifically, after the dyeing process is completed, the pressure relief valves are opened in sequence to recover the carbon dioxide in the system and to separate the residual dye. After the system cools to room temperature and the pressure returns to normal, the lid 4 is opened and the dyeing shaft 7 is taken out to complete the experimental operation.

[0123] Furthermore, the dyeing method also includes measuring the temperature of the outer wall of the dyeing vessel 2 using a thermocouple digital thermometer during the dyeing cycle.

[0124] Furthermore, to verify the accuracy of the simulation results, both a dyeing vessel without a spiral flow guide structure and the dyeing vessel of the present invention with a spiral flow guide structure were selected and subjected to actual dyeing operations under the same operating conditions as the simulation settings. Temperature measurements were simultaneously performed during the dyeing cycle to compare the differences in temperature distribution on the outer wall of the vessel under the two structures during actual operation, thereby verifying the credibility of the simulation results.

[0125] The final temperature measurement results show that in the dyeing kettle without a flow guiding structure, the maximum temperature difference on the outer wall of the dyeing kettle reaches 13℃, indicating a significant temperature unevenness. However, in the dyeing kettle of the present invention with a spiral flow guiding structure, the maximum temperature difference on the outer wall of the kettle can be reduced to less than 3℃, and the temperature field distribution is more uniform, which is highly consistent with the simulation analysis results. This further verifies the accuracy of the simulation model and the effectiveness of the spiral flow guiding structure in improving the thermal field uniformity.

[0126] The supercritical carbon dioxide anhydrous dyeing kettle, dyeing system, and dyeing method provided by this invention incorporate a spiral guide plate within the jacket. Simulation analysis shows that this structure significantly extends the flow path of the heat transfer medium within the jacket, ensuring its uniform distribution on the outer wall of the dyeing chamber. This enhances the contact and convection between the medium and the heat exchange surface, thereby reducing the maximum temperature difference on the outer wall of the dyeing kettle from 13°C to 3°C. This prevents thermal damage issues such as color spots and fiber melting caused by localized overheating or excessive temperature differences.

[0127] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

Claims

1. A supercritical anhydrous dyeing vessel, characterized in that, The dyeing vessel includes at least: The dyeing vessel body (2) includes a closed end and an open end, and the dyeing vessel body (2) is provided with a dyeing chamber (1) inside; The lid (4) is fixedly connected to the open end of the dyeing vessel body (2) and the open end is closed. Heating and cooling jacket device (5), the heating and cooling jacket device (5) is sleeved and fixed on the outside of the dyeing kettle body (2), the heating and cooling jacket device (5) is a hollow structure, and a medium with heating or cooling function is introduced into the inside; The dyeing warp shaft (7) is located in the middle of the dyeing chamber (1) of the dyeing vessel body (2). The dyeing warp shaft (7) is a hollow tube, and multiple fluid permeation holes (6) are opened on the tube wall of the dyeing warp shaft (7). The heating and cooling jacket device (5) is also provided with a spiral flow guiding structure, which is arranged along the outer wall of the dyeing kettle body (2). The heating and cooling jacket device (5) has a multi-layer cylindrical structure between the jacket and the dyeing vessel body (2).

2. The supercritical anhydrous dyeing vessel according to claim 1, characterized in that, The spiral guide structure is a spiral guide plate (14), which is arranged in a spiral shape and is welded and fixed to the outer wall of the dyeing vessel body (2) in a spiral winding manner.

3. The supercritical anhydrous dyeing vessel according to claim 1, characterized in that, The heating and cooling jacket device (5) is also provided with a heat transfer medium inlet (9) and a heat transfer medium outlet (10). The heat transfer medium inlet (9) is arranged at one end of the heating and cooling jacket device (5) near the lid (4), and the heat transfer medium outlet (10) is arranged on the other side of the heating and cooling jacket device (5). The heat transfer medium inlet (9) and the heat transfer medium outlet (10) are located on the same side of the heating and cooling jacket device (5) and communicate with the internal space of the heating and cooling jacket device (5).

4. The supercritical anhydrous dyeing vessel according to claim 3, characterized in that, The dyeing vessel body (2) is also provided with a carbon dioxide outlet (12) and a carbon dioxide inlet (13). The carbon dioxide outlet (12) and the carbon dioxide inlet (13) are respectively connected to the dyeing chamber (1). The carbon dioxide outlet (12) is located on the outer wall of the dyeing vessel body (2) near the opening end and extends outward through the heating and cooling jacket device (5) to form an interface. The carbon dioxide inlet (13) is located at the closed end of the dyeing vessel body (2), is connected to one end of the dyeing shaft (7), and extends outward through the heating and cooling jacket device (5) to form an interface.

5. The supercritical anhydrous dyeing vessel according to claim 4, characterized in that, The dyeing vessel body (2) is provided with three carbon dioxide outlets (12). The three carbon dioxide outlets (12) are evenly spaced along the circumference, and the three carbon dioxide outlets (12) are collected by a flow collection structure and then connected to a pipe for recycling.

6. The supercritical anhydrous dyeing vessel according to claim 4, characterized in that, The two ends of the dyeing shaft (7) are respectively fixed with circular sealing baffles (8). The outer wall surface of the dyeing vessel (2) is also provided with a temperature measuring device (3) for measuring the temperature distribution data of the outer wall of the dyeing vessel (2). The temperature measuring device (3) includes multiple patch temperature sensors arranged along the axial direction of the dyeing vessel. A set of temperature measuring points is set in the upper, middle and lower regions of the vessel.

7. A supercritical carbon dioxide anhydrous staining system, characterized in that, The dyeing system includes the supercritical anhydrous dyeing kettle as described in any one of claims 1-6, and a carbon dioxide pressurization supply device, a color matching device, a circulation device, and a separation and recovery device, all of which are controlled by an automatic control system and connected to the supercritical anhydrous dyeing kettle. The staining system includes two supercritical anhydrous staining vessels (19), which are arranged in parallel. The pressurization time of the second supercritical anhydrous staining vessel (19) is reduced by equalizing the pressure.

8. The supercritical carbon dioxide anhydrous staining system according to claim 7, characterized in that, The carbon dioxide pressurization supply device includes a carbon dioxide storage tank (15), a pressurization pump (16), and a preheater 17; the color mixing device includes a color mixing vessel (18) and a dye box disposed inside the color mixing vessel (18); the dyeing device and the circulation device include at least one circulation pump (20) and at least one heat exchanger (21); the separation and recovery device includes a condenser (22), a multi-stage separation vessel (23), and a transfer pump (24); Among them, carbon dioxide passes through carbon dioxide storage tank (15), pressurizing pump (16) and preheater (17), and then enters color mixing kettle (18) through circulation pipe. The outlet of color mixing kettle (18) is connected to carbon dioxide inlet (13) of supercritical anhydrous dyeing kettle (19). Supercritical anhydrous dyeing kettle (19) is connected to circulation pump (20) and heat exchanger (21) through circulation pipe to form a dyeing circulation mechanism. The carbon dioxide circulation outlet of the supercritical anhydrous dyeing vessel (19) is connected to the condenser (22) to cool and depressurize the dye liquor after dyeing. Then, the carbon dioxide and dye are separated by the multi-stage separation vessel (23). Finally, the carbon dioxide is introduced into the carbon dioxide storage tank (15) by the transfer pump (24).

9. A staining method using a supercritical carbon dioxide anhydrous staining system, characterized in that, The staining method includes: Place the dyeing warp beam (7) with the fabric to be dyed wound around it into the supercritical anhydrous dyeing kettle as described in any one of claims 1-6, and place the dye into the color matching device; Carbon dioxide gas is introduced into the staining system, and the system is heated and pressurized to the set parameters; After the temperature and pressure in the dyeing system stabilize to the preset value, the circulation device is turned on to perform dyeing cycle until the specified dyeing time is reached. After dyeing is completed, the separation and recovery device is activated to recover the residual carbon dioxide medium in the system.

10. The staining method of the supercritical carbon dioxide anhydrous staining system according to claim 9, characterized in that, The dyeing method further includes measuring the temperature of the outer wall of the dyeing vessel (2) using a thermocouple digital thermometer during the dyeing cycle.

Citation Information

Patent Citations

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