Nylon supercritical carbon dioxide anhydrous splicing dyeing process and dye composition thereof

Abstract

The invention relates to the technical field of dyeing and finishing, and particularly discloses a supercritical carbon dioxide anhydrous splicing dyeing process for chinlon and a dye composition thereof, the dye composition is formed by mixing C.I. Disperse yellow 54 and C.I. Disperse red 60, or the dye composition is formed by mixing C.I. Disperse yellow 54 and C.I. Disperse blue 60. Stepwise heating is adopted in the pressurizing and heating step, circulating dyeing is divided into two stages, and the heating rate from the dyeing temperature of the first stage to the dyeing temperature of the second stage is controlled to be 0.5 DEG C / min-1. 0 DEG C / min. According to the invention, the disperse yellow 56, the disperse red 60 and the two combined dyes of the disperse yellow 56 and the disperse blue 60 with good compatibility are screened, the color matching leveling property is improved by controlling the heating rate, one-bath color matching of chinlon is realized in the supercritical CO2 fluid, the method has the characteristics of cleanness and low energy consumption, and the washing resistance and the dry and wet rubbing color fastness are all above level 3-4.

Description

Technical Field

[0001] This invention relates to the field of textile dyeing and finishing technology, specifically to a supercritical carbon dioxide anhydrous dyeing process for nylon and its dye composition. Background Technology

[0002] Nylon is a hydrophobic fiber containing amino and carboxyl groups, allowing it to be dyed with disperse and acid dyes. Its dyeing process is characterized by rapid dyeing rate and high exhaustion rate. However, nylon has a very low dye saturation value, making the competition between different dyes particularly prominent during blending dyeing. If the selected dye combinations differ significantly in dyeing rate and affinity, the resulting colors will vary considerably at different dyeing times, leading to uneven color distribution and poor reproducibility.

[0003] Supercritical CO2 dyeing boasts advantages such as a short dyeing cycle, no need for pretreatment or washing, and the recyclability of CO2 and dyes. The solubility and diffusion rate of dyes in the supercritical medium can be controlled by adjusting pressure and temperature. Therefore, compared to traditional water-based dyeing media, supercritical CO2 dyeing technology offers richer and more multi-dimensional process implementation solutions in terms of dyeing mechanisms and improving dyeing quality. It is of great significance for promoting cleaner production, energy conservation, and emission reduction in the dyeing industry.

[0004] Currently, research on supercritical CO2 dyed fabrics focuses on polyester, aramid, and natural fibers, with very few reports on nylon dyeing and no research on color matching for nylon. Summary of the Invention

[0005] The purpose of this invention is to provide a supercritical carbon dioxide anhydrous dyeing process for nylon and its dye composition, which can effectively improve the dyeing level of nylon and enrich the color of nylon dyeing without the need for the addition of auxiliaries, while causing less damage to the fabric. It can be used to dye textiles of various colors.

[0006] To achieve the above-mentioned objectives, the technical solution adopted by this invention is as follows: A supercritical carbon dioxide anhydrous dye composition for nylon, wherein the dye composition is a mixture of CI Disperse Yellow 54 and CI Disperse Red 60, or the dye composition is a mixture of CI Disperse Yellow 54 and CI Disperse Blue 60.

[0007] Preferably, the mixing ratio of CI Disperse Yellow 54 and CI Disperse Red 60 is 4:1, 3:1, 2:1, 1:1, 1:2, 1:3 or 1:4.

[0008] Preferably, the mixing ratio of CI Disperse Yellow 54 and CI Disperse Blue 60 is 4:1, 3:1, 2:1 or 1:1.

[0009] The present invention further provides a supercritical carbon dioxide anhydrous dyeing process for nylon, which specifically includes the following steps: S1. Loading: Place the nylon fabric in the dyeing kettle, mix the above dye composition evenly, place it in the dyeing kettle, and connect it to the dyeing circulation system; S2, Pressurization and Heating: Switch to pressurization and heating mode, and turn off after the temperature and pressure reach the set values. The heating is done in a stepped manner. S3, Circulating Dyeing: Switch to circulating dyeing mode, so that the dye composition in the dye tank is dissolved in supercritical carbon dioxide and then enters the dyeing tank and circulates back and forth; S4. Separation and Recovery: Switch to separation and recovery mode to separate and recover supercritical carbon dioxide from the dye composition. S5. Open the dyeing kettle and dye kettle, and take out the nylon dyed fabric and the remaining dye composition.

[0010] Preferably, in step S1, the dye composition is 0.1%-6% of the weight of the nylon fabric.

[0011] Preferably, in step S1, the dye composition is 0.1%-6% of the weight of the nylon fabric.

[0012] Preferably, the step heating in step S2 is divided into two stages, with the heating rate in the first stage being lower than that in the second stage.

[0013] Preferably, the heating rate in the first stage is 0.5℃ / min-1℃ / min, and the heating rate in the second stage is 2℃ / min-5℃ / min.

[0014] Preferably, the cyclic staining temperature in step S3 is 80℃-120℃, the pressure is 16MPa-24MPa, and the holding time is 20min-60min.

[0015] Preferably, the cyclic staining in step S3 is divided into two stages: the first stage has a temperature of 80℃-110℃, a pressure of 16MPa-24MPa, and a holding time of 20min-40min; the second stage has a temperature of 110℃-120℃, a pressure of 16MPa-24MPa, and a holding time of 20min-30min; and the heating rate from the staining temperature in the first stage to the staining temperature in the second stage is controlled at 0.5℃ / min-1.0℃ / min.

[0016] Compared with the prior art, the present invention has the following beneficial effects: This invention screened two dye combinations with good compatibility: Disperse Yellow 56 and Disperse Red 60, and Disperse Yellow 56 and Disperse Blue 60. By controlling the heating rate, the color matching and leveling properties were improved, and one-bath color matching of nylon was achieved in supercritical CO2 fluid, which has the characteristics of being clean and having low energy consumption.

[0017] According to GB / T 3920-2008 "Textiles - Tests for color fastness to rubbing" and GB / T 3921-2008 "Textiles - Tests for color fastness to rubbing: test", the nylon dyed fabric of this invention has a color fastness to washing and dry and wet rubbing of grade 3 or above, which meets the requirements of national standards. Detailed Implementation

[0018] Example 1 This embodiment provides a supercritical carbon dioxide anhydrous dyeing process for nylon, which specifically includes the following steps: S1. Loading: Place the PA 66 nylon fabric in the dyeing kettle, mix the dye composition thoroughly, place it in the dyeing kettle, and connect it to the dyeing circulation system. The dye composition is 1% of the weight of the nylon fabric, and the dye composition is a mixture of CI Disperse Yellow 54 and CI Disperse Red 60 in a mass ratio of 4:1.

[0019] S2. Pressurization and Heating: Switch to pressurization and heating mode, turn on the pressurization pump, inject carbon dioxide, and turn on the heat exchange device for step heating. Turn off the device after the temperature and pressure reach the set values. The heating is carried out in a step-heating manner, which is divided into two stages. The heating rate of the first stage is 0.5℃ / min, and the heating rate of the second stage is 2℃ / min.

[0020] S3. Circulating Dyeing: Switch to circulating dyeing mode. The dye composition in the dyeing tank dissolves in supercritical carbon dioxide and then enters the dyeing tank for repeated circulation. This is divided into two stages: the first stage has a temperature of 100℃, a pressure of 20MPa, and a holding time of 40min; the second stage has a temperature of 110℃, a pressure of 20MPa, and a holding time of 30min. The heating rate from the first stage dyeing temperature to the second stage dyeing temperature is controlled at 0.5℃ / min.

[0021] S4. Separation and Recovery: Switch to separation and recovery mode to separate and recover supercritical carbon dioxide from the dye composition.

[0022] S5. Open the dyeing kettle and dye kettle, take out the nylon dyed fabric and the remaining dye composition, and evaluate it according to GB / T 3920-2008 "Color fastness test of textiles - color fastness to rubbing" and GB / T 3921-2008 "Color fastness test of textiles - color fastness to washing: test". In this example, the nylon dyed fabric has a washing fastness of grade 4, a dry rubbing fastness of grade 4, a wet rubbing fastness of grade 4, and no color spots, and good even dyeing properties.

[0023] Example 2 This embodiment provides a supercritical carbon dioxide anhydrous dyeing process for nylon, which specifically includes the following steps: S1. Loading: Place the PA 66 nylon fabric in the dyeing kettle, mix the dye composition thoroughly, place it in the dyeing kettle, and connect it to the dyeing circulation system. The dye composition is 1% of the weight of the nylon fabric, and the dye composition is a mixture of CI Disperse Yellow 54 and CI Disperse Red 60 in a mass ratio of 3:1.

[0024] S2. Pressurization and Heating: Switch to pressurization and heating mode, turn on the pressurization pump, inject carbon dioxide, and turn on the heat exchange device for step heating. Turn off the device after the temperature and pressure reach the set values. The heating is carried out in a step-heating manner, which is divided into two stages. The heating rate of the first stage is 0.5℃ / min, and the heating rate of the second stage is 2℃ / min.

[0025] S3. Circulating Dyeing: Switch to circulating dyeing mode. The dye composition in the dyeing tank dissolves in supercritical carbon dioxide and then enters the dyeing tank for repeated circulation. This is divided into two stages: the first stage has a temperature of 95℃, a pressure of 20MPa, and a holding time of 30min; the second stage has a temperature of 110℃, a pressure of 20MPa, and a holding time of 30min. The heating rate from the first stage dyeing temperature to the second stage dyeing temperature is controlled at 0.5℃ / min.

[0026] S4. Separation and Recovery: Switch to separation and recovery mode to separate and recover supercritical carbon dioxide from the dye composition.

[0027] S5. Open the dyeing kettle and dye kettle, take out the nylon dyed fabric and the remaining dye composition, and evaluate it according to GB / T 3920-2008 "Color fastness test of textiles - color fastness to rubbing" and GB / T 3921-2008 "Color fastness test of textiles - color fastness to washing: test". In this example, the nylon dyed fabric has a washing fastness of grade 4, a dry rubbing fastness of grade 4, a wet rubbing fastness of grade 4, and no color spots, and good even dyeing properties.

[0028] Example 3 This embodiment provides a supercritical carbon dioxide anhydrous dyeing process for nylon, which specifically includes the following steps: S1. Loading: Place the PA 66 nylon fabric in the dyeing kettle, mix the dye composition thoroughly, place it in the dyeing kettle, and connect it to the dyeing circulation system. The dye composition is 1% of the weight of the nylon fabric, and the dye composition is a mixture of CI Disperse Yellow 54 and CI Disperse Red 60 in a mass ratio of 2:1.

[0029] S2. Pressurization and Heating: Switch to pressurization and heating mode, turn on the pressurization pump, inject carbon dioxide, and turn on the heat exchange device for step heating. Turn off the device after the temperature and pressure reach the set values. The heating is carried out in a step-heating manner, which is divided into two stages. The heating rate of the first stage is 0.5℃ / min, and the heating rate of the second stage is 2℃ / min.

[0030] S3. Circulating Dyeing: Switch to circulating dyeing mode. The dye composition in the dyeing vessel dissolves in supercritical carbon dioxide and then enters the dyeing vessel for repeated circulation. This is divided into two stages: the first stage has a temperature of 100℃, a pressure of 20MPa, and a holding time of 30min; the second stage has a temperature of 110℃, a pressure of 20MPa, and a holding time of 20min. The heating rate from the first stage dyeing temperature to the second stage dyeing temperature is controlled at 0.5℃ / min.

[0031] S4. Separation and Recovery: Switch to separation and recovery mode to separate and recover supercritical carbon dioxide from the dye composition.

[0032] S5. Open the dyeing kettle and dye kettle, take out the nylon dyed fabric and the remaining dye composition, and evaluate it according to GB / T 3920-2008 "Color fastness test of textiles - color fastness to rubbing" and GB / T 3921-2008 "Color fastness test of textiles - color fastness to washing: test". In this example, the nylon dyed fabric has a washing fastness of grade 4, a dry rubbing fastness of grade 4, a wet rubbing fastness of grade 4, and no color spots, and good even dyeing properties.

[0033] Example 4 This embodiment provides a supercritical carbon dioxide anhydrous dyeing process for nylon, which specifically includes the following steps: S1. Loading: Place the PA 66 nylon fabric in the dyeing kettle, mix the dye composition thoroughly, place it in the dyeing kettle, and connect it to the dyeing circulation system. The dye composition is 1% of the weight of the nylon fabric, and the dye composition is a mixture of CI Disperse Yellow 54 and CI Disperse Red 60 in a mass ratio of 1:1.

[0034] S2. Pressurization and Heating: Switch to pressurization and heating mode, turn on the pressurization pump, inject carbon dioxide, and turn on the heat exchange device for step heating. Turn off the device after the temperature and pressure reach the set values. The heating is carried out in a step-heating manner, which is divided into two stages. The heating rate of the first stage is 0.5℃ / min, and the heating rate of the second stage is 2℃ / min.

[0035] S3. Circulating Dyeing: Switch to circulating dyeing mode. The dye composition in the dyeing vessel dissolves in supercritical carbon dioxide and then enters the dyeing vessel for repeated circulation. This is divided into two stages: the first stage has a temperature of 100℃, a pressure of 20MPa, and a holding time of 20min; the second stage has a temperature of 110℃, a pressure of 20MPa, and a holding time of 20min. The heating rate from the first stage dyeing temperature to the second stage dyeing temperature is controlled at 0.5℃ / min.

[0036] S4. Separation and Recovery: Switch to separation and recovery mode to separate and recover supercritical carbon dioxide from the dye composition.

[0037] S5. Open the dyeing kettle and dye kettle, take out the nylon dyed fabric and the remaining dye composition, and evaluate it according to GB / T 3920-2008 "Color fastness test of textiles - color fastness to rubbing" and GB / T 3921-2008 "Color fastness test of textiles - color fastness to washing: test". In this example, the nylon dyed fabric has a washing fastness of grade 4, a dry rubbing fastness of grade 4, a wet rubbing fastness of grade 4, and no color spots, and good even dyeing properties.

[0038] Example 5 This embodiment provides a supercritical carbon dioxide anhydrous dyeing process for nylon, which specifically includes the following steps: S1. Loading: Place the PA 66 nylon fabric in the dyeing kettle, mix the dye composition thoroughly, place it in the dyeing kettle, and connect it to the dyeing circulation system. The dye composition is 1% of the weight of the nylon fabric, and the dye composition is a mixture of CI Disperse Yellow 54 and CI Disperse Blue 60 in a mass ratio of 4:1.

[0039] S2. Pressurization and Heating: Switch to pressurization and heating mode, turn on the pressurization pump, inject carbon dioxide, and turn on the heat exchange device for step heating. Turn off the device after the temperature and pressure reach the set values. The heating is carried out in a step-heating manner, which is divided into two stages. The heating rate of the first stage is 0.5℃ / min, and the heating rate of the second stage is 2℃ / min.

[0040] S3. Circulating Dyeing: Switch to circulating dyeing mode. The dye composition in the dyeing tank dissolves in supercritical carbon dioxide and then enters the dyeing tank for repeated circulation. This is divided into two stages: the first stage has a temperature of 100℃, a pressure of 20MPa, and a holding time of 40min; the second stage has a temperature of 110℃, a pressure of 20MPa, and a holding time of 30min. The heating rate from the first stage dyeing temperature to the second stage dyeing temperature is controlled at 0.5℃ / min.

[0041] S4. Separation and Recovery: Switch to separation and recovery mode to separate and recover supercritical carbon dioxide from the dye composition.

[0042] S5. Open the dyeing kettle and dye kettle, take out the nylon dyed fabric and the remaining dye composition, and evaluate it according to GB / T 3920-2008 "Color fastness test of textiles - color fastness to rubbing" and GB / T 3921-2008 "Color fastness test of textiles - color fastness to washing: test". In this example, the nylon dyed fabric has a washing fastness of grade 4, a dry rubbing fastness of grade 4, a wet rubbing fastness of grade 4, and no color spots, and good even dyeing properties.

[0043] Example 6 This embodiment provides a supercritical carbon dioxide anhydrous dyeing process for nylon, which specifically includes the following steps: S1. Loading: Place the PA 66 nylon fabric in the dyeing kettle, mix the dye composition thoroughly, place it in the dyeing kettle, and connect it to the dyeing circulation system. The dye composition is 1% of the weight of the nylon fabric, and the dye composition is a mixture of CI Disperse Yellow 54 and CI Disperse Blue 60 in a mass ratio of 3:1.

[0044] S2. Pressurization and Heating: Switch to pressurization and heating mode, turn on the pressurization pump, inject carbon dioxide, and turn on the heat exchange device for step heating. Turn off the device after the temperature and pressure reach the set values. The heating is carried out in a step-heating manner, which is divided into two stages. The heating rate of the first stage is 0.5℃ / min, and the heating rate of the second stage is 2℃ / min.

[0045] S3. Circulating Dyeing: Switch to circulating dyeing mode. The dye composition in the dyeing tank dissolves in supercritical carbon dioxide and then enters the dyeing tank for repeated circulation. This is divided into two stages: the first stage has a temperature of 100℃, a pressure of 20MPa, and a holding time of 30min; the second stage has a temperature of 110℃, a pressure of 20MPa, and a holding time of 30min. The heating rate from the first stage dyeing temperature to the second stage dyeing temperature is controlled at 0.5℃ / min.

[0046] S4. Separation and Recovery: Switch to separation and recovery mode to separate and recover supercritical carbon dioxide from the dye composition.

[0047] S5. Open the dyeing kettle and dye kettle, take out the nylon dyed fabric and the remaining dye composition, and evaluate it according to GB / T 3920-2008 "Color fastness test of textiles - color fastness to rubbing" and GB / T 3921-2008 "Color fastness test of textiles - color fastness to washing: test". In this example, the nylon dyed fabric has a washing fastness of grade 4, a dry rubbing fastness of grade 4, a wet rubbing fastness of grade 4, and no color spots, and good even dyeing properties.

[0048] Example 7 This embodiment provides a supercritical carbon dioxide anhydrous dyeing process for nylon, which specifically includes the following steps: S1. Loading: Place the PA 66 nylon fabric in the dyeing kettle, mix the dye composition thoroughly, place it in the dyeing kettle, and connect it to the dyeing circulation system. The dye composition is 1% of the weight of the nylon fabric, and the dye composition is a mixture of CI Disperse Yellow 54 and CI Disperse Blue 60 in a mass ratio of 2:1.

[0049] S2. Pressurization and Heating: Switch to pressurization and heating mode, turn on the pressurization pump, inject carbon dioxide, and turn on the heat exchange device for step heating. Turn off the device after the temperature and pressure reach the set values. The heating is carried out in a step-heating manner, which is divided into two stages. The heating rate of the first stage is 0.5℃ / min, and the heating rate of the second stage is 2℃ / min.

[0050] S3. Circulating Dyeing: Switch to circulating dyeing mode. The dye composition in the dyeing vessel dissolves in supercritical carbon dioxide and then enters the dyeing vessel for repeated circulation. This is divided into two stages: the first stage has a temperature of 100℃, a pressure of 20MPa, and a holding time of 30min; the second stage has a temperature of 110℃, a pressure of 20MPa, and a holding time of 20min. The heating rate from the first stage dyeing temperature to the second stage dyeing temperature is controlled at 0.5℃ / min.

[0051] S4. Separation and Recovery: Switch to separation and recovery mode to separate and recover supercritical carbon dioxide from the dye composition.

[0052] S5. Open the dyeing kettle and dye kettle, take out the nylon dyed fabric and the remaining dye composition, and evaluate it according to GB / T 3920-2008 "Color fastness test of textiles - color fastness to rubbing" and GB / T 3921-2008 "Color fastness test of textiles - color fastness to washing: test". In this example, the nylon dyed fabric has a washing fastness of grade 4, a dry rubbing fastness of grade 4, a wet rubbing fastness of grade 4, and no color spots, and good even dyeing properties.

[0053] Example 8 This embodiment provides a supercritical carbon dioxide anhydrous dyeing process for nylon, which specifically includes the following steps: S1. Loading: Place the PA 66 nylon fabric in the dyeing kettle, mix the dye composition thoroughly, place it in the dyeing kettle, and connect it to the dyeing circulation system. The dye composition is 1% of the weight of the nylon fabric, and the dye composition is a mixture of CI Disperse Yellow 54 and CI Disperse Blue 60 in a mass ratio of 1:1.

[0054] S2. Pressurization and Heating: Switch to pressurization and heating mode, turn on the pressurization pump, inject carbon dioxide, and turn on the heat exchange device for step heating. Turn off the device after the temperature and pressure reach the set values. The heating is carried out in a step-heating manner, which is divided into two stages. The heating rate of the first stage is 0.5℃ / min, and the heating rate of the second stage is 2℃ / min.

[0055] S3. Circulating Dyeing: Switch to circulating dyeing mode. The dye composition in the dyeing vessel dissolves in supercritical carbon dioxide and then enters the dyeing vessel for repeated circulation. This is divided into two stages: the first stage has a temperature of 100℃, a pressure of 20MPa, and a holding time of 20min; the second stage has a temperature of 110℃, a pressure of 20MPa, and a holding time of 20min. The heating rate from the first stage dyeing temperature to the second stage dyeing temperature is controlled at 0.5℃ / min.

[0056] S4. Separation and Recovery: Switch to separation and recovery mode to separate and recover supercritical carbon dioxide from the dye composition.

[0057] S5. Open the dyeing kettle and dye kettle, take out the nylon dyed fabric and the remaining dye composition, and evaluate it according to GB / T 3920-2008 "Color fastness test of textiles - color fastness to rubbing" and GB / T 3921-2008 "Color fastness test of textiles - color fastness to washing: test". In this example, the nylon dyed fabric has a washing fastness of grade 4, a dry rubbing fastness of grade 4, a wet rubbing fastness of grade 4, and no color spots, and good even dyeing properties.

[0058] Example 9 This embodiment provides a supercritical carbon dioxide anhydrous dyeing process for nylon, which specifically includes the following steps: S1. Loading: Place the PA 66 nylon fabric in the dyeing kettle, mix the dye composition thoroughly, place it in the dyeing kettle, and connect it to the dyeing circulation system. The dye composition is 1% of the weight of the nylon fabric, and the dye composition is a mixture of CI Disperse Yellow 54 and CI Disperse Red 60 in a mass ratio of 1:1.

[0059] S2. Pressurization and Heating: Switch to pressurization and heating mode, turn on the pressurization pump, inject carbon dioxide, and turn on the heat exchange device for step heating. Turn off the device after the temperature and pressure reach the set values. The heating is carried out in a step-heating manner, which is divided into two stages. The heating rate of the first stage is 1℃ / min, and the heating rate of the second stage is 2℃ / min.

[0060] S3. Circulating Dyeing: Switch to circulating dyeing mode. The dye composition in the dyeing vessel dissolves in supercritical carbon dioxide and then enters the dyeing vessel for repeated circulation. This is divided into two stages: the first stage has a temperature of 110℃, a pressure of 20MPa, and a holding time of 20min; the second stage also has a temperature of 110℃, a pressure of 20MPa, and a holding time of 20min. The heating rate from the first stage to the second stage is controlled at 1.0℃ / min.

[0061] S4. Separation and Recovery: Switch to separation and recovery mode to separate and recover supercritical carbon dioxide from the dye composition.

[0062] S5. Open the dyeing kettle and dye kettle, take out the nylon dyed fabric and the remaining dye composition, and evaluate it according to GB / T 3920-2008 "Color fastness test of textiles - color fastness to rubbing" and GB / T 3921-2008 "Color fastness test of textiles - color fastness to washing: test". In this example, the nylon dyed fabric has a washing fastness of grade 4, a dry rubbing fastness of grade 4, a wet rubbing fastness of grade 3-4, and no color spots, and good even dyeing properties.

[0063] Example 10 This embodiment provides a supercritical carbon dioxide anhydrous dyeing process for nylon, which specifically includes the following steps: S1. Loading: Place the PA 66 nylon fabric in the dyeing kettle, mix the dye composition thoroughly, place it in the dyeing kettle, and connect it to the dyeing circulation system. The dye composition is 1% of the weight of the nylon fabric, and the dye composition is a mixture of CI Disperse Yellow 54 and CI Disperse Red 60 in a mass ratio of 1:1.

[0064] S2. Pressurization and Heating: Switch to pressurization and heating mode, turn on the pressurization pump, inject carbon dioxide, and turn on the heat exchange device for step heating. Turn off the device after the temperature and pressure reach the set values. The heating is carried out in a step-heating manner, which is divided into two stages. The heating rate of the first stage is 1℃ / min, and the heating rate of the second stage is 3℃ / min.

[0065] S3. Circulating Dyeing: Switch to circulating dyeing mode. The dye composition in the dyeing vessel dissolves in supercritical carbon dioxide and then enters the dyeing vessel for repeated circulation. This is divided into two stages: the first stage has a temperature of 100℃, a pressure of 20MPa, and a holding time of 20min; the second stage has a temperature of 110℃, a pressure of 20MPa, and a holding time of 20min. The heating rate from the first stage dyeing temperature to the second stage dyeing temperature is controlled at 1.0℃ / min.

[0066] S4. Separation and Recovery: Switch to separation and recovery mode to separate and recover supercritical carbon dioxide from the dye composition.

[0067] S5. Open the dyeing kettle and dye kettle, take out the nylon dyed fabric and the remaining dye composition, and evaluate it according to GB / T 3920-2008 "Color fastness test of textiles - color fastness to rubbing" and GB / T 3921-2008 "Color fastness test of textiles - color fastness to washing: test". In this example, the nylon dyed fabric has a washing fastness of grade 4, a dry rubbing fastness of grade 4, a wet rubbing fastness of grade 3-4, and no color spots, and good even dyeing properties.

[0068] Example 11 This embodiment provides a supercritical carbon dioxide anhydrous dyeing process for nylon, which specifically includes the following steps: S1. Loading: Place the PA 66 nylon fabric in the dyeing kettle, mix the dye composition thoroughly, place it in the dyeing kettle, and connect it to the dyeing circulation system. The dye composition is 1% of the weight of the nylon fabric, and the dye composition is a mixture of CI Disperse Yellow 54 and CI Disperse Red 60 in a mass ratio of 1:1.

[0069] S2. Pressurization and Heating: Switch to pressurization and heating mode, turn on the pressurization pump, inject carbon dioxide, and turn on the heat exchange device for step heating. Turn off the device after the temperature and pressure reach the set values. The heating is carried out in a step-heating manner, which is divided into two stages. The heating rate of the first stage is 1℃ / min, and the heating rate of the second stage is 5℃ / min.

[0070] S3. Circulating Dyeing: Switch to circulating dyeing mode. The dye composition in the dyeing vessel dissolves in supercritical carbon dioxide and then enters the dyeing vessel for repeated circulation. This is divided into two stages: the first stage has a temperature of 100℃, a pressure of 20MPa, and a holding time of 20min; the second stage has a temperature of 110℃, a pressure of 20MPa, and a holding time of 20min. The heating rate from the first stage dyeing temperature to the second stage dyeing temperature is controlled at 1.0℃ / min.

[0071] S4. Separation and Recovery: Switch to separation and recovery mode to separate and recover supercritical carbon dioxide from the dye composition.

[0072] S5. Open the dyeing kettle and dye kettle, take out the nylon dyed fabric and the remaining dye composition, and evaluate it according to GB / T 3920-2008 "Color fastness test of textiles - color fastness to rubbing" and GB / T 3921-2008 "Color fastness test of textiles - color fastness to washing: test". In this example, the color fastness of the nylon dyed fabric to washing is grade 3-4, the color fastness to dry rubbing is grade 3-4, the color fastness to wet rubbing is grade 3-4, and there is no color spot and the dyeing uniformity is good.

[0073] Example 12 This embodiment provides a supercritical carbon dioxide anhydrous dyeing process for nylon, which specifically includes the following steps: S1. Loading: Place the PA 66 nylon fabric in the dyeing kettle, mix the dye composition thoroughly, place it in the dyeing kettle, and connect it to the dyeing circulation system. The dye composition is 1% of the weight of the nylon fabric, and the dye composition is a mixture of CI Disperse Yellow 54 and CI Disperse Blue 60 in a mass ratio of 1:1.

[0074] S2. Pressurization and Heating: Switch to pressurization and heating mode, turn on the pressurization pump, inject carbon dioxide, and turn on the heat exchange device for step heating. Turn off the device after the temperature and pressure reach the set values. The heating is carried out in a step-heating manner, which is divided into two stages. The heating rate of the first stage is 1℃ / min, and the heating rate of the second stage is 3℃ / min.

[0075] S3. Circulating Dyeing: Switch to circulating dyeing mode. The dye composition in the dyeing vessel dissolves in supercritical carbon dioxide and then enters the dyeing vessel for repeated circulation. This is divided into two stages: the first stage has a temperature of 100℃, a pressure of 20MPa, and a holding time of 20min; the second stage has a temperature of 110℃, a pressure of 20MPa, and a holding time of 20min. The heating rate from the first stage dyeing temperature to the second stage dyeing temperature is controlled at 1.0℃ / min.

[0076] S4. Separation and Recovery: Switch to separation and recovery mode to separate and recover supercritical carbon dioxide from the dye composition.

[0077] S5. Open the dyeing kettle and dye kettle, take out the nylon dyed fabric and the remaining dye composition, and evaluate it according to GB / T 3920-2008 "Color fastness test of textiles - color fastness to rubbing" and GB / T 3921-2008 "Color fastness test of textiles - color fastness to washing: test". In this example, the color fastness of the nylon dyed fabric to washing is grade 3-4, the color fastness to dry rubbing is grade 4, and the color fastness to wet rubbing is grade 3-4. It also has no color spots and good evenness.

[0078] Example 13 This embodiment provides a supercritical carbon dioxide anhydrous dyeing process for nylon, which specifically includes the following steps: S1. Loading: Place the PA 66 nylon fabric in the dyeing kettle, mix the dye composition thoroughly, place it in the dyeing kettle, and connect it to the dyeing circulation system. The dye composition is 1% of the weight of the nylon fabric, and the dye composition is a mixture of CI Disperse Yellow 54 and CI Disperse Blue 60 in a mass ratio of 1:1.

[0079] S2. Pressurization and Heating: Switch to pressurization and heating mode, turn on the pressurization pump, inject carbon dioxide, and turn on the heat exchange device for step heating. Turn off the device after the temperature and pressure reach the set values. The heating is carried out in a step-heating manner, which is divided into two stages. The heating rate of the first stage is 1℃ / min, and the heating rate of the second stage is 5℃ / min.

[0080] S3. Circulating Dyeing: Switch to circulating dyeing mode. The dye composition in the dyeing vessel dissolves in supercritical carbon dioxide and then enters the dyeing vessel for repeated circulation. This is divided into two stages: the first stage has a temperature of 100℃, a pressure of 20MPa, and a holding time of 20min; the second stage has a temperature of 110℃, a pressure of 20MPa, and a holding time of 20min. The heating rate from the first stage dyeing temperature to the second stage dyeing temperature is controlled at 1.0℃ / min.

[0081] S4. Separation and Recovery: Switch to separation and recovery mode to separate and recover supercritical carbon dioxide from the dye composition.

[0082] S5. Open the dyeing kettle and dye kettle, take out the nylon dyed fabric and the remaining dye composition, and evaluate it according to GB / T 3920-2008 "Color fastness test of textiles - color fastness to rubbing" and GB / T 3921-2008 "Color fastness test of textiles - color fastness to washing: test". In this example, the color fastness of the nylon dyed fabric to washing is grade 3-4, the color fastness to dry rubbing is grade 3-4, the color fastness to wet rubbing is grade 3-4, and there is no color spot and the dyeing uniformity is good.

[0083] Comparative Example 1 This embodiment provides a supercritical carbon dioxide anhydrous dyeing process for nylon, which specifically includes the following steps: S1. Loading: Place the PA 66 nylon fabric in the dyeing kettle, mix the dye composition thoroughly, place it in the dyeing kettle, and connect it to the dyeing circulation system. The dye composition is 1% of the weight of the nylon fabric, and the dye composition is a mixture of CI Disperse Yellow 54 and CI Disperse Blue 60 in a mass ratio of 1:1.

[0084] S2. Pressurization and Heating: Switch to pressurization and heating mode, turn on the pressurization pump, inject carbon dioxide, and turn on the heat exchange device for step heating. Turn off the device after the temperature and pressure reach the set values. The heating is carried out in a step-heating manner, which is divided into two stages. The heating rate of the first stage is 1℃ / min, and the heating rate of the second stage is 5℃ / min.

[0085] S3. Circulating Dyeing: Switch to circulating dyeing mode. The dye composition in the dyeing vessel dissolves in supercritical carbon dioxide and then enters the dyeing vessel for repeated circulation. This is divided into two stages: the first stage has a temperature of 100℃, a pressure of 20MPa, and a holding time of 20min; the second stage has a temperature of 110℃, a pressure of 20MPa, and a holding time of 20min. The heating rate from the first stage dyeing temperature to the second stage dyeing temperature is controlled at 2.0℃ / min.

[0086] S4. Separation and Recovery: Switch to separation and recovery mode to separate and recover supercritical carbon dioxide from the dye composition.

[0087] S5. Open the dyeing kettle and dye kettle, take out the nylon dyed fabric and the remaining dye composition, and evaluate it according to GB / T 3920-2008 "Color fastness test of textiles - color fastness to rubbing" and GB / T 3921-2008 "Color fastness test of textiles - color fastness to washing: test". In this example, the color fastness of the nylon dyed fabric to washing is grade 3, the color fastness to dry rubbing is grade 3-4, the color fastness to wet rubbing is grade 3, and there is no color spotting and the dyeing uniformity is good.

[0088] Comparative Example 2 This comparative example provides a supercritical carbon dioxide anhydrous dyeing process for nylon, which specifically includes the following steps: S1. Loading: Place the PA 66 nylon fabric in the dyeing kettle, mix the dye composition thoroughly, place it in the dyeing kettle, and connect it to the dyeing circulation system. The dye composition is 1% of the weight of the nylon fabric, and the dye composition is a mixture of CI Disperse Yellow 54 and CI Disperse Red 60 in a mass ratio of 3:1.

[0089] S2. Pressurization and Heating: Switch to pressurization and heating mode, turn on the pressurization pump, inject carbon dioxide, and turn on the heat exchange device for step heating. Turn off the device after the temperature and pressure reach the set values. The heating is carried out in a step-heating manner, which is divided into two stages. The heating rate of the first stage is 0.5℃ / min, and the heating rate of the second stage is 2℃ / min.

[0090] S3. Circulating dyeing: Switch to circulating dyeing mode, so that the dye composition in the dyeing tank is dissolved in supercritical carbon dioxide and then enters the dyeing tank and circulates back and forth. The parameters are consistent throughout the process. The circulating dyeing temperature is 110℃, the pressure is 20MPa, and the holding time is 60min.

[0091] S4. Separation and Recovery: Switch to separation and recovery mode to separate and recover supercritical carbon dioxide from the dye composition.

[0092] S5. Open the dyeing kettle and dye kettle, take out the nylon dyed fabric and the remaining dye composition, and evaluate it according to GB / T 3920-2008 "Textiles - Tests for Color Fastness to Rubbing" and GB / T 3921-2008 "Textiles - Tests for Color Fastness to Washing: Test". In this example, the color fastness of the nylon dyed fabric to washing is grade 3, the color fastness to dry rubbing is grade 3-4, the color fastness to wet rubbing is grade 3, and a few color spots appear.

[0093] The foregoing has shown and described the basic principles, main features and advantages of this invention. Those skilled in the art should understand that this invention is not limited to the above embodiments. The embodiments and descriptions in the specification are only illustrative of the principles of this invention. Various changes and modifications can be made to this invention without departing from the spirit and scope of this invention. All such changes and modifications fall within the scope of this invention as claimed. The scope of protection of this invention is defined by the appended claims and their equivalents.

Claims

1. A supercritical carbon dioxide anhydrous dye composition for nylon, characterized in that: The dye composition is a mixture of CI Disperse Yellow 54 and CI Disperse Red 60, or the dye composition is a mixture of CI Disperse Yellow 54 and CI Disperse Blue 60.

2. The nylon supercritical carbon dioxide anhydrous dye composition according to claim 1, characterized in that: The mixing ratio of CI Disperse Yellow 54 and CI Disperse Red 60 is 4:1, 3:1, 2:1, 1:1, 1:2, 1:3 or 1:

4.

3. The nylon supercritical carbon dioxide anhydrous dye composition according to claim 1, characterized in that: The mixing ratio of CI Disperse Yellow 54 and CI Disperse Blue 60 is 4:1, 3:1, 2:1 or 1:

1.

4. A supercritical carbon dioxide anhydrous dyeing process for nylon, characterized in that, Specifically, the steps include the following: S1. Loading: Place the nylon fabric in the dyeing kettle, mix the dye composition as described in any one of claims 1 to 3, place it in the dyeing kettle, and connect it to the dyeing circulation system; S2, Pressurization and Heating: Switch to pressurization and heating mode, and turn off after the temperature and pressure reach the set values. The heating is done in a stepped manner. S3, Circulating Dyeing: Switch to circulating dyeing mode, so that the dye composition in the dye tank is dissolved in supercritical carbon dioxide and then enters the dyeing tank and circulates back and forth; S4. Separation and Recovery: Switch to separation and recovery mode to separate and recover supercritical carbon dioxide from the dye composition. S5. Open the dyeing kettle and dye kettle, and take out the nylon dyed fabric and the remaining dye composition.

5. The nylon supercritical carbon dioxide anhydrous dyeing process according to claim 4, characterized in that: In step S1, the dye composition is 0.1%-6% of the weight of the nylon fabric.

6. The supercritical carbon dioxide anhydrous dyeing process for nylon according to claim 5, characterized in that: In step S1, the dye composition is 0.1%-6% of the weight of the nylon fabric.

7. The supercritical carbon dioxide anhydrous dyeing process for nylon according to claim 1, characterized in that: The step heating in step S2 is divided into two stages, with the heating rate in the first stage being lower than that in the second stage.

8. The supercritical carbon dioxide anhydrous dyeing process for nylon according to claim 7, characterized in that: The heating rate in the first stage is 0.5℃ / min-1℃ / min, and the heating rate in the second stage is 2℃ / min-5℃ / min.

9. The supercritical carbon dioxide anhydrous dyeing process for nylon according to claim 1, characterized in that: In step S3, the cyclic staining temperature is 80℃-120℃, the pressure is 16MPa-24MPa, and the holding time is 20min-60min.

10. The supercritical carbon dioxide anhydrous dyeing process for nylon according to claim 9, characterized in that: The cyclic staining in step S3 is divided into two stages. The first stage has a temperature of 80℃-110℃, a pressure of 16MPa-24MPa, and a holding time of 20min-40min. The second stage has a temperature of 110℃-120℃, a pressure of 16MPa-24MPa, and a holding time of 20min-30min. The heating rate from the staining temperature in the first stage to the staining temperature in the second stage is controlled at 0.5℃ / min-1.0℃ / min.