Non-aqueous solvent active dyeing method for wool and / or cashmere product
By using a non-aqueous solvent reactive dyeing method, the problems of low utilization rate and low fixation rate of reactive dyes in the dyeing of wool and cashmere products have been solved, realizing an efficient and water-saving dyeing process that maintains the luster and color fastness of the products.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-26
- Publication Date
- 2026-04-10
AI Technical Summary
Existing reactive dyeing methods for wool and cashmere have low utilization rates and low fixation rates of reactive dyes. The processes are complex, water consumption is high, and frequent pH adjustments and high-temperature washing are required, which leads to yellowing, shrinkage, and loss of luster in the products.
The non-aqueous solvent reactive dyeing method is adopted, which mixes wool and cashmere products with reactive dyes, retarder and good solvent, controls temperature and solvent ratio, avoids pH adjustment and high temperature washing, and achieves efficient dyeing and fixation of reactive dyes.
It improves the utilization and fixation rate of reactive dyes, reduces water consumption, avoids yellowing and shrinkage of products, maintains gloss, and has a shorter dyeing time and better color fastness than traditional methods.
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to a non-aqueous solvent active dyeing method of wool and / or cashmere containing products, and belongs to the field of textile dyeing and finishing technology. BACKGROUND
[0002] The active dyeing of wool (cashmere) is a process of forming a covalent bond between active dyes and amino groups in wool (cashmere) fibers. In traditional water bath wool (cashmere) active dyeing, the following shortcomings exist:
[0003] Firstly, the selectivity of active dyes is small and the fixation rate is low. For existing wool (cashmere) specific active dyes on the market (such as Lanasol series), although they have a high fixation rate (90-95%), their price is high and the variety is small, and production enterprises often choose other cotton active dyes as substitutes, but the fixation rate after dyeing is often lower (60-80%). Low fixation rate also causes problems such as large water consumption and long process time in post-processing.
[0004] Secondly, in traditional wool (cashmere) active dyeing, the pH value of the dye bath needs to be accurately controlled. Usually, maintaining weak acidity (such as pH value of 4-6) in the dyeing stage is beneficial to dye adsorption; and in the fixation stage, the pH value needs to be adjusted to near neutral (such as pH value of 5.5-7.0) to promote the formation of covalent bonds. Frequent pH adjustment brings the disadvantages of complex process, poor stability, long time consumption, and also consumes a large amount of pH adjuster: such as acetic acid, sodium acetate, ammonium sulfate, ammonia, soda ash, etc.
[0005] In addition, in the existing non-aqueous solvent active dyeing method for protein fibers, the product containing protein fibers (such as loose fibers, yarns, fabrics or clothes, etc.) needs to be treated with alkali and swelling in an alkaline solution. However, the product containing wool (cashmere) and other protein fibers is treated with water in an alkaline condition before active dyeing, which has high fixation rate, but produces obvious yellowing, shrinkage, and loss of surface luster.
[0006] Therefore, it has become a technical problem to be solved in the field to provide a non-aqueous solvent active dyeing method of wool and / or cashmere containing products, which realizes the dyeing and fixation of active dyes on wool and / or cashmere containing products without using acid and alkali adjusters, high-temperature cleaning, and alkali pretreatment. SUMMARY
[0007] In order to solve the above-mentioned shortcomings and deficiencies, the purpose of the present application is to provide a non-aqueous solvent active dyeing method for wool and / or cashmere products. The present application can at least solve the problems of low utilization rate of reactive dyes, low fixation rate, complex process and large water consumption in post-processing of the traditional water bath process for dyeing wool and / or cashmere products.
[0008] In order to achieve the above-mentioned purpose, in one aspect, the present application provides a non-aqueous solvent active dyeing method for wool and / or cashmere products, wherein the method comprises:
[0009] Step (1): mixing wool and / or cashmere products with a mixed solution containing reactive dyes, a dyeing retardant and a good solvent for reactive dyes to form a mixed system; adding a poor solvent for reactive dyes to the mixed system before and / or during the heating process, heating to 60-80℃ and dyeing; wherein the volume ratio of the good solvent for reactive dyes to the poor solvent for reactive dyes is 1:(1-2.8);
[0010] Step (2): continuing to heat to 80-100℃ to fix the wool and / or cashmere products;
[0011] Step (3): washing the wool and / or cashmere products after fixing.
[0012] As a specific embodiment of the above-mentioned method of the present application, the wool and / or cashmere products include loose fibers, yarns, fabrics or garments, etc. Accordingly, the dyeing methods include loose fiber dyeing, yarn dyeing, piece dyeing, garment dyeing, etc.
[0013] As a specific embodiment of the above-mentioned method of the present application, the weight ratio of the wool and / or cashmere products to the good solvent for reactive dyes is 1:(2-8).
[0014] As a specific embodiment of the above-mentioned method of the present application, the dyeing retardant is cardanol polyoxyethylene ether, including one or a combination of BGF-5, BGF-6, BGF-7, etc.
[0015] As a specific embodiment of the above-mentioned method of the present application, the amount of the dyeing retardant is 0.5-2% of the weight of the wool and / or cashmere products.
[0016] The amount of reactive dyes used in the above-mentioned method of the present application is not specifically required and can be reasonably adjusted according to the needs of dyeing.
[0017] As a specific embodiment of the above-mentioned method of the present application, the good solvent for the reactive dye is a polar solvent capable of dissolving the reactive dye but not chemically reacting with the reactive dye, including one or a combination of N,N-dimethylformamide, N,N-dimethylacetamide, dimethyl sulfoxide, ionic liquid, and alcoholic ether solvent.
[0018] As a specific embodiment of the above-mentioned method of the present application, the poor solvent for the reactive dye is a solvent incapable of dissolving the reactive dye and not chemically reacting with the reactive dye, including one or a combination of chlorinated or non-chlorinated hydrocarbon (such as alkane, alkene, and aromatic hydrocarbon, etc.) solvent, silane solvent, ketone solvent, ester solvent, and ether solvent.
[0019] As a specific embodiment of the above-mentioned method of the present application, the poor solvent for the reactive dye includes one or a combination of C6-C8 n-alkane, C6-C8 iso-alkane, tetrachloroethylene, trichloroethylene, decamethylcyclopentasiloxane (D5), and dimethyl carbonate.
[0020] As a specific embodiment of the above-mentioned method of the present application, the method further includes recycling the solvent, and the recycling mode includes one or a combination of delamination, decolorization, and distillation.
[0021] In the above-mentioned method of the present application, the poor solvent for the reactive dye can be miscible with the good solvent for the reactive dye after being heated, and the good solvent for the reactive dye loses its solubility for the reactive dye after being miscible and is more distributed on the fabric. By adjusting the volume ratio of the good solvent for the reactive dye to the poor solvent for the reactive dye and the system temperature, the dyeing speed and degree can be controlled. Specifically, the volume ratio of the good solvent for the reactive dye to the poor solvent for the reactive dye is controlled to be 1:(1-2.8), and the dyeing degree is significantly improved.
[0022] As a specific embodiment of the above-mentioned method of the present application, in step (1), the poor solvent for the reactive dye can be added in batches during the heating process, and the present application does not make specific requirements for the specific number of batches, which can be reasonably adjusted as needed as long as the purpose of the present application can be achieved.
[0023] As a specific embodiment of the above-mentioned method of the present application, in steps (1) and (2), the heating rate of the heating is 0.5-5℃ / min.
[0024] As a specific embodiment of the above-mentioned method of the present application, in step (1), the parent type of the reactive dye includes one or a combination of anthraquinone type, azo type, phthalocyanine type and metal complex type.
[0025] And / or, the active group type of the reactive dye includes one or a combination of ethylene sulfone, halogenated s-triazine, nicotinamide, etc.
[0026] As a specific embodiment of the above-mentioned method of the present application, in step (2), the time for fixing is 15-60 min.
[0027] As a specific embodiment of the above-mentioned method of the present application, in step (3), the washing includes room temperature washing.
[0028] On the other hand, the present application also provides a wool and / or cashmere product dyed with a reactive dye, which is obtained by the above-mentioned non-aqueous solvent reactive dyeing method of the wool and / or cashmere product.
[0029] Compared with the prior art, the present application can achieve at least the following beneficial technical effects:
[0030] The method provided by the present application uses a non-aqueous solvent to perform reactive dyeing on a wool and / or cashmere product, and the target product can be obtained after simple water washing of the dyed product. The up-dyeing and fixing processes do not require the use of acid and alkali adjusting agents to adjust the pH, and do not require high-temperature washing. The method has the characteristics of high utilization rate of reactive dyes and high fixing rate, and solves the problems of low utilization rate of reactive dyes for traditional water dyeing of wool and / or cashmere products, frequent adjustment of pH, and the need for a large amount of water for washing in post-processing.
[0031] The method provided by the present application does not require alkalization and swelling treatment of the wool and / or cashmere product in an alkaline solution before dyeing, and the product will not yellow, shrink, or lose surface gloss.
[0032] In the method provided by the present application, all solvents can be recycled and reused after use, and the recovery rate can reach 99.5%.
[0033] In summary, the method provided by the present application can realize high up-dyeing and high fixing of reactive dyes on wool and / or cashmere products by using a non-aqueous solvent as a medium, without the use of acid and alkali adjusting agents to adjust the pH, high-temperature washing, and alkaline agent pretreatment. Compared with the conventional water dyeing process, the dyeing time of the method is comparable, water consumption can be saved by 75%, the fixing rate can be increased to more than 95%, and the color fastness of the obtained product is comparable to or better than that of the product obtained by conventional water dyeing. DETAILED DESCRIPTION
[0034] It has to be understood that the term "comprising", and any variation thereof, as used in the description and the claims of the present application, is intended to cover not only the listed steps or units but also any process, method, system, product, or apparatus that comprises those steps or units, without necessarily being limited to the precise steps or units thereof.
[0035] The ranges disclosed herein are given using the format "from about 'lower limit' to about 'upper limit'." The terms "about" and "approximately" can be used interchangeably herein to indicate that a value is intended to be within a range of values that one of ordinary skill in the art would accept as the precision with which an actual value need not be taken. For example, a range of 60-120 and 80-110 is understood to include ranges of 60-110 and 80-120, respectively. In addition, a range of 1-3, 1-4, 1-5, 2-3, 2-4, and 2-5 is understood to be contemplated if a minimum range value of 1 and 2 is listed, and a maximum range value of 3, 4, and 5 is listed.
[0036] In the present application, unless otherwise stated, the numerical range "a-b" indicates a shorthand for the inclusion of any integer or combination of integers between a and b, where a and b are both real numbers. For example, the numerical range "0-5" indicates that all real numbers between "0-5" have been listed in the present application, and "0-5" is merely a shorthand for these numerical combinations.
[0037] In the present application, all the embodiments and preferred embodiments mentioned in the present application can be combined with each other to form new technical solutions, if not otherwise specified.
[0038] In the present application, all the technical features and preferred features mentioned in the present application can be combined with each other to form new technical solutions, if not otherwise specified.
[0039] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used in the description of the application herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used herein, the term "and / or" includes any and all combinations of one or more of the associated listed items.
[0040] In order to make the objectives, technical solutions and advantages of the present application clearer, the present application will be further described in detail below in combination with embodiments. The following described embodiments are part of the embodiments of the present application, rather than all the embodiments, and are only used to illustrate the present application, and should not be regarded as limiting the scope of the present application. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative labor fall within the scope of protection of the present application. If the specific conditions are not specified in the embodiments, the conventional conditions or the conditions recommended by the manufacturer are used. If the reagents or instruments used are not specified by the manufacturer, they are all conventional products that can be purchased on the market.
[0041] Example 1
[0042] The present embodiment provides a non-aqueous solvent active dyeing method for wool knitted fabric, wherein the method comprises the following specific steps:
[0043] Step (1): Take 10 g of wool knitted fabric and put it into a dye cup, take 0.3 g (3% o.w.f) of LANASOL RED B and 0.1 g of cardanol polyoxyethylene ether (BGF-6), and dissolve them in 60 mL of dimethyl sulfoxide to obtain a mixed solution, add the mixed solution to the dye cup, start the dye solution circulation, enter the dyeing at 40℃, start the temperature rise, adjust the temperature rise rate to 1℃ / min and rise to 70℃ at this temperature rise rate, and add 120 mL of trichloroethylene in batches during the temperature rise process, and keep the temperature at 70℃ for a certain period of time until the dyeing rate reaches equilibrium, at this time the dyeing rate is measured to be 99.7%.
[0044] Step (2): Continue to rise at a temperature rise rate of 1℃ / min to 95℃ and keep for 40 min until the dyeing is complete.
[0045] Step (3): After wringing the solvent in the wool knitted fabric, take it out, and then perform water washing at room temperature to complete the non-aqueous solvent active dyeing of the wool knitted fabric, and the dyeing rate is measured to be 98.7%, and the obtained dyed wool knitted fabric still has the natural soft hand feeling and luster of wool, and the longitudinal shrinkage is measured to be 12%.
[0046] Select four points on the surface of the dyed wool knitted fabric, compare them in pairs, and test the △E with a Datacolor 650 tester, and the maximum △E is 0.64 and the average △E value is 0.41.
[0047] Again, the dyed wool knitted fabric obtained in Example 1 is tested for fastness by using the existing conventional fastness test method in the art, and the test results are as follows:
[0048] The dry rubbing is 4.0 grade, the wet rubbing is 3.5 grade, the water washing color change is 4.5 grade, and the water washing staining is 4.5 grade.
[0049] The reference standard of dry friction and wet friction is GB / T 3920, the index requirements in the standard are 4.0 grade (dry grinding) and ≥3.0 grade (wet grinding, dark color 2.0) respectively, the reference standard of water washing discoloration and water washing staining is GB / T 3922, the index requirements in the standard are ≥4.0 grade (discoloration) and ≥3.0 grade (staining) respectively. The fastness test standards and index requirements in other examples and comparative examples are the same as those in example 1.
[0050] It can be seen that the dyed wool knitted fabric obtained by example 1 has high color fixation rate and excellent color fastness.
[0051] Comparative example 1
[0052] The present comparative example provides a water-solvent active dyeing method of wool knitted fabric, wherein the method comprises the following specific steps:
[0053] Dyeing: take 10g of wool knitted fabric and put it into a dye cup, take 0.3g (3% o.w.f) of LANASOL REDB and dissolve it in 120mL of water to obtain a dyeing solution, first add 1g / L of penetrant LCF-185 to the dyeing solution, stir uniformly, then add 1.2g / L of glacial acetic acid to the dyeing solution to adjust the pH of the dyeing solution to 4.5, and then add the obtained mixed solution to the dye cup, dye at room temperature, start heating, adjust the heating rate to 1℃ / min and heat to 95℃ at the heating rate, and keep the temperature for 60min; after the dyeing step is completed, the dyeing rate is measured to be 93%.
[0054] Ammonia washing and color fixation: take 40g of 20wt% ammonia water and dissolve it in 960g of water, at this time the pH value of the system is 11.3, to obtain an ammonia water working solution, take the dyed wool knitted fabric obtained in the above step and 120mL of the ammonia water working solution and add them to the dye cup, heat to 80℃ and keep the temperature for 20min, drain the water, and the color fixation step is completed. Take the residual liquid to determine the dye concentration.
[0055] Hot water washing: take the ammonia washing and color fixation wool knitted fabric obtained in the above step and 120mL of clean water and add them to the dye cup, heat to 80℃ and keep the temperature for 10min, drain the water. Take the residual liquid to determine the dye concentration.
[0056] Cold water washing: take the hot water washing wool knitted fabric obtained in the above step and 120mL of clean water and add them to the dye cup, run at room temperature for 10min, drain the water. Take the residual liquid to determine the dye concentration.
[0057] After all the above procedures are completed, the color fixation rate is calculated to be 92.5%.
[0058] The dyed wool knitted fabric obtained in comparative example 1 is subjected to fastness test by using the conventional fastness test method in the prior art, and the test results are as follows:
[0059] The dry friction is 4.0, the wet friction is 3.0, the water washing discoloration is 4.5, and the water washing staining is 4.5.
[0060] According to the experimental results of the comparative example 1 and the comparative example 1, the wool knitted fabric is subjected to active dyeing by using the non-aqueous solvent in the example 1 of the present application, and the finished product can be obtained after simple water washing of the wool knitted fabric after dyeing, without high-temperature cleaning, so that the dye fixation rate is higher, and the problems of low utilization rate of active dyes, frequent pH adjustment, and high-temperature cleaning with a large amount of water after dyeing in the prior art water-solvent active dyeing method are solved. In addition, the method provided in the example of the present application can make the dyes fully dye without adjusting the pH value, and the total water amount can be saved by 75%; the dye utilization rate is high, and the dye is saved. At the same time, compared with the finished product obtained in the comparative example 1, the wet friction of the finished product obtained in the example 1 of the present application is more excellent.
[0061] Comparative Example 2
[0062] The present comparative example provides a non-aqueous solvent active dyeing method for wool knitted fabric, wherein the method comprises the following specific steps:
[0063] 10 g of wool knitted fabric is taken and placed in a dye cup, a working solution containing 20 g / L of pure alkali and 1 g / L of penetrant LCF-185 is added to the dye cup, and the operation is carried out at 60℃ for 20 min; the wool knitted fabric is taken out and dried, at this time it is observed that the wool knitted fabric is yellow, shrinks seriously, and the hand feeling is obviously hardened.
[0064] The wool knitted fabric treated in the above step is placed in a dye cup, 0.3 g (3% o.w.f) of LANASOL RED B and 0.1 g of cardanol polyoxyethylene ether (BGF-6) are taken, and the two are dissolved in 60 mL of dimethyl sulfoxide to obtain a mixed solution, the mixed solution is added to the dye cup, the dye solution circulation is started, dyeing is started at 40℃, the temperature is increased at a rate of 1℃ / min, and the temperature is increased to 70℃ at the rate, 120 mL of trichloroethylene is added in batches during the temperature increasing process, and the temperature is kept at 70℃ for a certain time until the dyeing rate of the dye reaches equilibrium, at this time the dyeing rate is measured to be 99.6%.
[0065] The temperature is continued to increase at a rate of 1℃ / min to 95℃ and kept for 40 min until the fixation is complete.
[0066] After the solvent in the wool knitted fabric is wrung out, it is taken out, and water washing is carried out at room temperature, the non-aqueous solvent active dyeing of the wool knitted fabric is completed, and the fixation rate is measured to be 94.5%. It is found that the wool knitted fabric after dyeing in the comparative example 2 shrinks seriously, the longitudinal shrinkage rate is as high as 30%, and the natural soft hand feeling and luster of wool are lost.
[0067] Compared with Comparative Example 2, the method provided by Inventive Example 1 does not use an alkali agent to pretreat the wool knitted fabric before dyeing. Accordingly, the finished product obtained by Inventive Example 1 is significantly better than the finished product obtained by Comparative Example 2 in terms of fixation rate, fabric hand feeling, gloss, and size (reflected by longitudinal shrinkage).
[0068] Comparative Example 3
[0069] This comparative example provides a non-aqueous solvent reactive dyeing method for wool knitted fabric, wherein the method comprises the following specific steps:
[0070] Step (1): Take 10 g of wool knitted fabric and place it in a dye cup. Take 0.3 g (3% o.w.f) of LANASOL RED B and 0.1 g of cardanol polyoxyethylene ether (BGF-6), and dissolve them in 60 mL of dimethyl sulfoxide to obtain a mixed solution. Add the mixed solution to the dye cup, start the dye solution circulation, and dye at 40°C. Start the temperature rise, adjust the temperature rise rate to 1°C / min, and rise to 70°C at this temperature rise rate. Add 180 mL of trichloroethylene in batches during the temperature rise process, and keep the temperature at 70°C for a certain period of time until the dyeing rate reaches equilibrium. At this time, the dyeing rate is measured to be 99.6%.
[0071] Step (2): Continue to rise to 95°C at a temperature rise rate of 1°C / min and keep the temperature for 40 min until the fixation is complete.
[0072] Step (3): After wringing out the solvent in the wool knitted fabric, take it out and perform water washing at room temperature to complete the non-aqueous solvent reactive dyeing of the wool knitted fabric. The fixation rate is measured to be 98.8%.
[0073] Select four points on the surface of the dyed wool knitted fabric, compare them in pairs, and test the △E using a Datacolor 650 tester. The maximum △E obtained is 1.24, and the average △E value is 1.0.
[0074] Comparative Example 4
[0075] This comparative example provides a non-aqueous solvent reactive dyeing method for wool knitted fabric, wherein the method comprises the following specific steps:
[0076] Step (1): Take 10 g of wool knitted fabric and put it into a dye cup, take 0.3 g (3% o.w.f) of LANASOL RED B and 0.1 g of cardanol polyoxyethylene ether (BGF-6), and dissolve them in 60 mL of dimethyl sulfoxide to obtain a mixed solution, then add the mixed solution to the dye cup, start the dye solution circulation, dye at 40℃, start the temperature rise, adjust the temperature rise rate to 1℃ / min and rise to 70℃ at this temperature rise rate, and add 1800 mL of trichloroethylene in batches during the temperature rise process, and keep the temperature at 70℃ for a certain period of time until the dyeing rate reaches equilibrium, at this time the dyeing rate is measured to be 99.9%.
[0077] Step (2): Continue to rise at a temperature rise rate of 1℃ / min to 95℃ and keep for 40 min until the fixation is complete.
[0078] Step (3): After wringing out the solvent in the wool knitted fabric, take it out, and then wash it at room temperature to complete the non-aqueous solvent active dyeing of the wool knitted fabric, and the fixation rate is measured to be 99.1%.
[0079] Select four points on the surface of the dyed wool knitted fabric, compare them in pairs, and test the △E value with a Datacolor 650 tester, the maximum △E is 2.02, and the average △E value is 1.5.
[0080] Comparative Example 3 and Comparative Example 4 differ from Example 1 only in that the amount of trichloroethylene is 180 mL and 1800 mL, respectively, and the volume ratio of the good solvent of the reactive dye and the poor solvent of the reactive dye is 1:3 and 1:30, respectively. By comparing the experimental results of Comparative Example 3 and Comparative Example 4 with Example 1, although the dyeing rates and fixation rates of the three are comparable, the average △E values of the dyed wool knitted fabric obtained by Comparative Example 3 and Comparative Example 4 are not less than 1.0, which is significantly greater than that of the dyed wool knitted fabric obtained by Example 1, indicating that the dyed wool knitted fabric obtained by Example 1 has better level dyeing than Comparative Example 3 and Comparative Example 4, thereby proving that the method provided by the present application controls the volume ratio of the good solvent of the reactive dye and the poor solvent of the reactive dye to be 1:(1-2.8), which can significantly improve the level dyeing.
[0081] Example 2
[0082] The present embodiment provides a non-aqueous solvent active dyeing method for wool loose fibers, wherein the method comprises the following specific steps:
[0083] Step (1): Take 10 kg of wool loose fibers and put them into a dye cage, then hang the dye cage into a dyeing cylinder, and pre-charge 100 L of trichloroethylene into the main cylinder of the dyeing cylinder, and start the main pump to run to wet the wool loose fibers;
[0084] Take 300g (3% o.w.f) of Aircel RED SE and 0.1 kg of cardanol polyoxyethylene ether (BGF-6) and dissolve them in 60 L of dimethyl sulfoxide to obtain a mixed solution, and under the temperature condition of 40℃, the mixed solution is pumped into the main cylinder at a rate of 70% (i.e. 70% of the rated maximum feeding rate of the Dosing system) through the Dosing system;
[0085] Turn on the temperature rise, adjust the temperature rise rate to 1℃ / min, and rise to 55℃ at the temperature rise rate, add 50 L of tetrachloroethylene during the temperature rise, and keep the temperature at 55℃ for a certain period of time until the dyeing rate of the dye reaches equilibrium.
[0086] Step (2): again rise to 90℃ at a temperature rise rate of 1℃ / min and keep the temperature for 15 min; then drain, pressure dewatering, and control the liquor retention rate to be 150%, and then transfer the dyeing cage to the drying machine for solvent recovery.
[0087] Step (3): again transfer the dyeing cage to the yarn dyeing cylinder, add water, and wash the wool fibers at room temperature, complete the non-aqueous solvent active dyeing of the wool fibers, and measure the fixation rate of the dyed wool fibers to be 98.7%.
[0088] The dyed wool fibers obtained in Example 2 are tested for color fastness by using the conventional color fastness test method in the art, and the test results are as follows:
[0089] The dry rubbing is 4.0, the wet rubbing is 3.5, the water washing color change is 4.5, and the water washing color transfer is 4.5.
[0090] As can be seen, the dyed wool fibers obtained in Example 2 also have high fixation rate and excellent color fastness.
[0091] Example 3
[0092] The present embodiment provides a non-aqueous solvent active dyeing method for cashmere fibers, wherein the method comprises the following specific steps:
[0093] Step (1): take 13 kg of cashmere fibers and put them into a dyeing cage, then hang the dyeing cage into a yarn dyeing cylinder, pre-add 130 L of dimethyl carbonate to the main cylinder of the yarn dyeing cylinder, and start the main pump to run to wet the cashmere fibers;
[0094] Take 130g (1% o.w.f) of Aircel GOLD SE and 0.1 kg of cardanol polyoxyethylene ether (BGF-7) and dissolve them in 80 L of dimethyl sulfoxide to obtain a mixed solution, and under the temperature condition of 40℃, the mixed solution is pumped into the main cylinder at a rate of 70% (i.e. 70% of the rated maximum feeding rate of the Dosing system) through the Dosing system;
[0095] Start to increase the temperature, adjust the temperature increasing rate to 1℃ / min and increase the temperature to 60℃ at the rate, add 80L of dimethyl carbonate during the temperature increasing process, keep the temperature at 60℃ for a certain time until the dyeing rate reaches equilibrium.
[0096] Step (2): increase the temperature to 95℃ at the rate of 1℃ / min and keep the temperature for 1 hour; then, carry out liquid discharge, pressure liquid discharge, and control the liquid retention rate to be 140%, and then transfer the dyeing cage to the drying machine for solvent recovery.
[0097] Step (3): transfer the dyeing cage to the yarn dyeing cylinder again, add water and carry out room temperature water washing on the cashmere fiber, complete the non-aqueous solvent active dyeing of the cashmere fiber, and measure that the fixation rate of the dyed cashmere fiber reaches 95.3%.
[0098] The dyed cashmere fiber obtained in Example 3 is subjected to fastness test by using the conventional fastness test method in the art, and the test results are as follows:
[0099] The dry rubbing is 4.0, the wet rubbing is 3.0, the water washing color change is 4.5, and the water washing staining is 4.5.
[0100] As can be seen, the dyed cashmere fiber obtained in Example 3 also has high fixation rate and excellent color fastness.
[0101] Example 4
[0102] The embodiment provides a non-aqueous solvent active dyeing method of wool yarn, and the method comprises the following specific steps:
[0103] Step (1): process 40 pieces of wool yarn into 1 kg specification of cheese, take 25 cheeses and hang them into the yarn dyeing cylinder, pre-add 190L of tetrachloroethylene to the main cylinder of the yarn dyeing cylinder, and start the main pump to run to wet the cheese;
[0104] Take 1000g (4% o.w.f) of black SE and 0.4 kg of cardanol polyoxyethylene ether (BGF-7), and dissolve the two in 100L of dimethyl sulfoxide to obtain a mixed solution, and the mixed solution is uniformly pumped into the main cylinder by the Dosing system under the condition of 35℃.
[0105] Start to increase the temperature, adjust the temperature increasing rate to 1℃ / min and increase the temperature to 50℃ at the rate, add 60L of tetrachloroethylene during the temperature increasing process, keep the temperature at 50℃ for a certain time until the dyeing rate reaches equilibrium.
[0106] Step (2): again increase the temperature to 95°C at a temperature increasing rate of 1°C / min and keep for 40 min; then carry out liquid discharge, pressure liquid discharge, and control the liquid retention rate to be 145%, and then transfer the dyeing cage to the drying machine for solvent recovery.
[0107] Step (3): again transfer the dyeing cage to the yarn dyeing cylinder, add clean water, and carry out room temperature water washing on the wool yarn, to complete the non-aqueous solvent active dyeing of the wool yarn. The fixation rate of the dyed wool yarn is measured to be 98.5%, the average ΔE value (measured by a Datacolor 650 tester) of the color difference between the outermost layer and the innermost layer of the cone is 0.4, the inner-outer difference is up to the standard, the appearance of the cone has no color ring and color mottle, and the level dyeing and penetration are good.
[0108] The dyed wool yarn obtained in Example 4 is subjected to fastness testing by using the conventional fastness testing method in the art, and the obtained testing results are as follows:
[0109] The dry rubbing is 4.5, the wet rubbing is 3.5, the washing color change is 4.5, and the washing color staining is 4.5.
[0110] Comparative Example 5
[0111] The present comparative example provides a non-aqueous solvent active dyeing method of wool yarn, wherein the method comprises the following specific steps:
[0112] Step (1): 40 wool yarns are processed into 1 kg specification cone yarns, 25 cones are taken and hung into the yarn dyeing cylinder, 190 L of tetrachloroethylene is pre-added to the main cylinder of the yarn dyeing cylinder, and the main pump is started to run to wet the cone yarns;
[0113] 1000 g (4% o.w.f) of black SE is taken and dissolved in 100 L of dimethyl sulfoxide to obtain a mixed solution, and the mixed solution is uniformly pumped into the main cylinder by the Dosing system at a temperature of 35°C;
[0114] Start to increase the temperature, adjust the temperature increasing rate to 1°C / min, and increase the temperature to 50°C at the temperature increasing rate, 60 L of tetrachloroethylene is added during the temperature increasing process, and keep the temperature at 50°C for a certain time until the dyeing rate of the dye reaches equilibrium.
[0115] Step (2): again increase the temperature to 95°C at a temperature increasing rate of 1°C / min and keep for 40 min; then carry out liquid discharge, pressure liquid discharge, and control the liquid retention rate to be 145%, and then transfer the dyeing cage to the drying machine for solvent recovery.
[0116] Step (3): again transfer the dyeing cage to the yarn dyeing cylinder, add clean water, and carry out room temperature water washing on the wool yarn, to complete the non-aqueous solvent active dyeing of the wool yarn.
[0117] Comparative Example 4 and Comparative Example 5 differ only in that no cardanol polyoxyethylene ether is used in Comparative Example 5.
[0118] The color fixation rate of the dyed wool yarn in Comparative Example 5 is also measured to be 98.5%, the same as in Example 4, and although the bobbin has no color circle and color mottle, the average ΔE value (measured by a Datacolor 650 tester) of the color difference between the outermost layer and the innermost layer of the bobbin is 0.8, higher than that of the dyed wool yarn obtained in Example 4, indicating that the level dyeing and penetration of the dyed wool yarn obtained in Comparative Example 5 are poorer than that of the dyed wool yarn obtained in Example 4, further indicating that the addition of cardanol polyoxyethylene ether can improve the level dyeing and penetration of the wool yarn in non-aqueous solvent active dyeing.
[0119] The fastness of the dyed wool yarn obtained in Comparative Example 5 is tested by using the conventional fastness test method in the art, and the test results are as follows:
[0120] The dry rubbing is 4.5, the wet rubbing is 3.5, the water washing color change is 4.5, and the water washing staining is 4.5. It can be seen that the color fastness of the dyed wool yarn in Comparative Example 5 and Example 4 is the same.
[0121] The above is only a specific embodiment of the present application, which cannot limit the scope of the application. Therefore, the replacement of equivalent components or equivalent changes and modifications made within the scope of the present patent protection should still fall within the scope of the present patent. In addition, the technical features in the present application can be freely combined with each other, and the technical features can be freely combined with each other.
Claims
1. A non-aqueous solvent active dyeing method of wool and / or cashmere containing products, characterized in that, The method comprises: Step (1): mixing the wool and / or cashmere containing product with a mixed solution containing reactive dyes, a dyeing retardant and a good solvent of the reactive dyes to form a mixed system; the mixed system is heated, and a poor solvent of the reactive dyes is added to the mixed system before and / or during the heating, and the temperature is raised to 60-80°C and the dyeing is performed; wherein the volume ratio of the good solvent of the reactive dyes to the poor solvent of the reactive dyes is 1:(1-2.8); Step (2): continuing to heat to 80-100°C to fix the color of the wool and / or cashmere containing product; Step (3): washing the wool and / or cashmere containing product after the fixing of the color.
2. The method of claim 1, wherein, The wool and / or cashmere containing product includes loose fibers, yarns, fabrics or garments.
3. The method according to claim 1 or 2, characterized in that, The weight ratio of the wool and / or cashmere containing product to the good solvent of the reactive dyes is 1:(2-8).
4. The method of claim 1, wherein, The dyeing retardant is cardanol polyoxyethylene, including one or a combination of BGF-5, BGF-6 and BGF-7.
5. The method according to any of claims 1-2, 4, characterized in that, The amount of the dyeing retardant is 0.5-2% of the weight of the wool and / or cashmere containing product.
6. The method according to any of claims 1-2, 4, characterized in that, The good solvent of the reactive dyes is a polar solvent that can dissolve the reactive dyes but does not chemically react with the reactive dyes, including one or a combination of N,N-dimethylformamide, N,N-dimethylacetamide, dimethyl sulfoxide, ionic liquid and alcohol ether solvent; And / or, the poor solvent of the reactive dyes is a solvent that cannot dissolve the reactive dyes and does not chemically react with the reactive dyes, including one or a combination of chlorinated or non-chlorinated hydrocarbon solvents, silane solvents, ketone solvents, ester solvents and ether solvents.
7. The method according to any of claims 1-2, 4, characterized by, In steps (1) and (2), the heating rate of the heating is 0.5-5°C / min.
8. The method according to any of claims 1-2, 4, characterized by, In step (1), the parent type of the reactive dyes includes one or a combination of anthraquinone type, azo type, phthalocyanine type and metal complex type; And / or, the active group type of the reactive dyes includes one or a combination of ethylene sulfone, halogenated s-triazine and nicotinamide.
9. The method according to any of claims 1-2, 4, characterized by, In step (2), the fixing time is 15-60 min.
10. A wool and / or cashmere containing product dyed with reactive dyes, which is obtained by the non-aqueous solvent reactive dyeing method of the wool and / or cashmere containing product according to any one of claims 1-9.