Microemulsion dyeing method
Through the microemulsion dyeing method, using a combination of reactive dyes, alkali slow-release agents and hydrophobic organic solvents, the problems of low dye utilization and wastewater pollution in traditional cotton fiber dyeing are solved, and efficient and clean dyeing effects are achieved.
Patent Information
- Application Number
- CN202510850926.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-24
- Publication Date
- 2025-10-17
AI Technical Summary
Traditional cotton fiber reactive dyeing has problems such as low exhaustion rate, low dye utilization rate, high degree of hydrolysis, and difficulty in removing hydrophobic solvents, which lead to uneven dyeing and serious wastewater pollution.
The microemulsion dyeing method is adopted, by mixing reactive dyes, alkali slow-release agents and hydrophobic organic solvent cyclopentyl methyl ether to form a microemulsion dye solution, using the alkali slow-release agent to gradually release alkaline substances to achieve salt-free dyeing, and removing the hydrophobic solvent through high-temperature baking to reduce the amount of detergent used.
The exhaustion rate and utilization rate of dyes are improved, the amount of chemical agents used is reduced, wastewater pollution is reduced, and clean dyeing of cellulose fibers is achieved.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of textile fabric, and particularly relates to a microemulsion dyeing method. BACKGROUND
[0002] Cotton fiber is a natural fiber, which has good moisture absorption, air permeability, natural skin-friendliness and other advantages, and is widely favored by consumers. The main component of cotton fiber is cellulose, so cotton fiber is mainly dyed with reactive dyes. In the traditional water medium reactive dyeing of cotton fiber, the cotton fiber first adsorbs the reactive dye in the dyeing solution without salt, and then salt such as sodium sulfate is added for dyeing promotion to improve the dye exhaustion rate. When the dyeing temperature rises to the target temperature, an alkali agent is added for fixation, and after a period of heat preservation, the temperature is lowered, washed, and the dyeing is completed. At the same time, the addition of alkali also increases the degree of hydrolysis of the reactive dye, reducing the use rate of the dye. Simply speaking, cotton fiber reactive dyeing requires salt for dyeing promotion and alkali for fixation.
[0003] In order to improve the dye exhaustion rate of reactive dyeing of cotton fiber, microemulsion dyeing technology has been adopted in recent years. First, a small amount of high-concentration dyeing solution is mixed with a hydrophobic organic solvent, and after high-speed stirring, the dyeing solution is uniformly distributed in the form of small droplets in the hydrophobic organic solvent to form a microemulsion dyeing system. Dry cotton fiber is immersed in the prepared microemulsion dyeing system. Since cotton fiber absorbs water, a small amount of water dyeing solution distributed in the microemulsion is efficiently adsorbed onto the cotton fiber, achieving a very high dye exhaustion rate, and even all the water solution is adsorbed, i.e. 100% dye exhaustion rate. Since alkali is required for the fixation of reactive dyeing of cotton fiber, if the alkali agent is added to the high-concentration dye to form a microemulsion dyeing system, it will cause a large amount of hydrolysis of the reactive dye. If the alkali agent is added after the dye exhaustion in the microemulsion dyeing process, such as adding solid alkali agent, the solid alkali agent cannot be dissolved in the microemulsion because the water medium in the microemulsion has been adsorbed by the cotton fiber, and the fixation of the reactive dye cannot be effectively completed. If an alkali solution is added, it introduces new water medium, which increases the water content in the microemulsion, so that the dye adsorbed on the cotton fiber is desorbed into the microemulsion, reducing the utilization rate of the dye. In addition, the cotton fiber is first treated with an alkali solution and then dried, i.e. the alkali is first treated on the cotton fiber to solve the problem of alkali fixation. However, adding a large amount of alkali agent on the cotton fiber before dyeing will also increase the hydrolysis of the dye, increasing the difficulty of the reproducibility of cotton fiber dyeing. In addition, during the microemulsion dyeing process, the hydrophobic solvent also adheres to the fiber, and more detergents need to be added and the washing times need to be increased to wash away the adhered hydrophobic solvent. SUMMARY
[0004] In order to overcome the above defects, the present application provides a microemulsion dyeing method, which can realize salt-free dyeing of cellulose fibers, improve the dye exhaustion rate and utilization rate, reduce the amount of chemicals for removing floating color, reduce the pollution of wastewater, and realize clean dyeing of cellulose fibers.
[0005] In order to achieve the above-mentioned purpose, the present application provides a microemulsion dyeing method, which comprises: 1) mixing a dyeing solution containing reactive dyes with an alkali agent slow-release agent, then mixing with a part of cyclopentyl methyl ether, then dropping the obtained mixed solution into the remaining part of cyclopentyl methyl ether to form a microemulsion dyeing solution, the water content of the microemulsion dyeing solution is 7-12 vol.%, the amount of the part of cyclopentyl methyl ether is 50-60 vol.% based on the total amount of cyclopentyl methyl ether, and the amount of the remaining part of cyclopentyl methyl ether is 40-50 vol.%; 2) immersing the pretreated cellulose fibers in the microemulsion dyeing solution, heating to 80-100℃ and keeping for 20-60 min, and then cooling to below 50℃.
[0006] Preferably, the water content of the microemulsion dyeing solution is 9-11 vol.%.
[0007] Preferably, the amount of the part of cyclopentyl methyl ether is 52-56 vol.% based on the total amount of cyclopentyl methyl ether, and the amount of the remaining part of cyclopentyl methyl ether is 44-48 vol.%.
[0008] Preferably, in the microemulsion dyeing solution, the amount of the reactive dyes is 1-5% (o.w.f), the amount of the alkali agent slow-release agent is 1-4% (o.w.f), and the content of the cyclopentyl methyl ether is 88-93 vol.%.
[0009] Preferably, the reactive dyes are at least one of nicotinic acid type reactive orange TCR-D, nicotinic acid type reactive orange TCR-5R and nicotinic acid type reactive red TCR-D.
[0010] Preferably, the alkali agent slow-release agent is at least one of AIO541, AIO533 and AIO500.
[0011] Preferably, in step 2), the bath ratio of the cellulose fibers to the microemulsion dyeing solution is 1:15-25.
[0012] Preferably, in step 2), the heating rate is 1-3℃ / min.
[0013] Preferably, in step 2), the cooling rate is 3-5℃ / min.
[0014] Preferably, the method further comprises: baking, soaping and drying the dyed material obtained after step 2) in sequence, wherein the baking conditions include: temperature of 110-140℃, and time of 10-20min.
[0015] The present application first prepares a microemulsion dyeing solution by mixing reactive dyes, a hydrophobic organic solvent cyclopentyl methyl ether, water and an alkali agent slow-release agent, and then uses the microemulsion dyeing solution to dye cellulose fibers, so that the high-efficiency adsorption of dyes in the reactive dyeing of cellulose fibers is realized, and the exhaustion rate can reach more than 90%, and at the same time, the salt-free dyeing of reactive dyes on cellulose fibers is realized. The use of the alkali agent slow-release agent can not only reduce the pre-dyeing alkali immersion process and shorten the dyeing process, but also reduce the hydrolysis of reactive dyes, improve the fixation efficiency and utilization rate of reactive dyes, thereby reducing the amount of chemical agents used for color washing and removal, and reducing the pollution of wastewater. When using nicotinic acid type reactive dyes for dyeing, the leaving group is a tertiary amine, which does not consume alkali, thereby reducing the amount of alkali used in the fixation process. The hydrophobic organic solvent in the microemulsion dyeing system, baking volatilization and washing wastewater in the present application can be recycled and reused, so that the clean dyeing of cellulose fibers is realized. DETAILED DESCRIPTION
[0016] The specific embodiments of the present application are described in detail below. It should be understood that the specific embodiments described herein are only used to illustrate and explain the present application, and are not used to limit the present application.
[0017] The endpoints of the ranges and any values disclosed herein are not limited to the precise values stated. The ranges or values should be construed to be approximations that allow for significant variation. Various ranges of values that are explicitly delineated between the endpoints, between a endpoint and a single value, and between single values, can be combined to form one or more new ranges of values that are also expressly disclosed.
[0018] The microemulsion dyeing method of the present application comprises: 1) mixing a dyeing solution containing reactive dyes with an alkali agent slow-release agent, then mixing with a part of cyclopentyl methyl ether, then adding the obtained mixed solution dropwise into the remaining part of cyclopentyl methyl ether to form a microemulsion dyeing solution, wherein the water content of the microemulsion dyeing solution is 7-12vol.%, the amount of the part of cyclopentyl methyl ether is 50-60vol.% based on the total amount of cyclopentyl methyl ether, and the amount of the remaining part of cyclopentyl methyl ether is 40-50vol.%; 2) immersing the pretreated cellulose fibers into the microemulsion dyeing solution, heating to 80-100℃ and keeping for 20-60min, and then cooling to below 50℃.
[0019] The microemulsion dyeing solution solves the problems of low dye exhaustion rate and uneven dyeing in traditional dyeing through the synergistic effect of "penetration-uniform adsorption", and provides a technical path for energy saving, consumption reduction, environmental protection and emission reduction.
[0020] The microemulsion dyeing solution of the application is a nanoscale micellar structure formed by an active dye-containing dyeing solution, a hydrophobic organic solvent cyclopentyl methyl ether and an alkali agent slow-release agent. The small droplets (100-800 nm) in the system can carry dye molecules to penetrate into the cellulose fiber more efficiently, reduce the aggregation of dyes on the fiber surface, and make the dye and fiber combination more firm, which has a significant effect on tight structure fibers.
[0021] In the microemulsion dyeing solution system, excessive water can exceed the saturation value of fiber water absorption, and then a large amount of unabsorbed water is dispersed in the microemulsion dyeing solution, which causes the dye adsorbed on the fiber to diffuse into the water of the microemulsion dyeing solution, reducing the amount of dye adsorbed on the fiber. At the same time, excessive water can cause part of the dye to adhere to the surface of the fiber, making it difficult to penetrate into the interior of the fiber, resulting in uneven dyeing of the cellulose fiber inside and outside. In step 1) of the microemulsion dyeing method of the application, the water content in the microemulsion dyeing solution can be further preferably 9-11 vol.%. The water content in the microemulsion dyeing solution system of the application is lower than that in the conventional microemulsion system, and the water phase is dispersed in the cyclopentyl methyl ether in the form of nanodroplets, avoiding micellar aggregation and reducing the penetration rate.
[0022] In order to promote the formation of the microemulsion dyeing solution, part of the cyclopentyl methyl ether is mixed with the dyeing solution containing active dyes and the alkali agent slow-release agent, and then the obtained mixed solution is added to the remaining part of the cyclopentyl methyl ether. In some embodiments, the amount of the part of the cyclopentyl methyl ether can be 52-56 vol.% based on the total amount of the cyclopentyl methyl ether, and the amount of the remaining part of the cyclopentyl methyl ether can be 44-48 vol.%. In some embodiments, 52-56 vol.% of cyclopentyl methyl ether is mixed with the dyeing solution containing active dyes and the alkali agent slow-release agent, and then the obtained mixed solution is added to the remaining 44-48 vol.% of cyclopentyl methyl ether. The cyclopentyl methyl ether is continuously stirred during the dropping process, the stirring speed is 8000-13000 rpm, the dropping speed of the mixed solution is 1 mL / 5 s-1 mL / 10 s, and the microemulsion dyeing solution is obtained. In the microemulsion dyeing solution, the small droplets can reach 100-200 nm.
[0023] In order to further promote the diffusion of the dye to the cellulose fiber and shorten the dyeing time, the amount of the reactive dye in the microemulsion dyeing solution of the present application can be 1-5% (o.w.f), preferably 2-3%, the amount of the alkali agent slow-release agent can be 1-4% (o.w.f), preferably 2-3%, and the content of the cyclopentyl methyl ether can be 88-93 vol.%, preferably 89-91 vol.%.
[0024] The reactive dye of the present application is not particularly limited, and in some embodiments, can be at least one of nicotinic acid type reactive orange TCR-D, nicotinic acid type reactive orange TCR-5R, and nicotinic acid type reactive red TCR-D, wherein the nicotinic acid type reactive orange TCR-D, the nicotinic acid type reactive orange TCR-5R, and the nicotinic acid type reactive red TCR-D are nicotinic acid type reactive dye products purchased from Wujiang Taoyuan Dyeing Co., Ltd.
[0025] The dyeing solution containing the reactive dye of the present application is to dissolve the reactive dye in water. In the microemulsion dyeing system, the concentration of the dyeing solution containing the reactive dye cooperates with the water content in the microemulsion dyeing system and the amount of each raw material to maintain the stability of the microemulsion dyeing system.
[0026] The alkali agent slow-release agent of the present application is gradually released in the microemulsion dyeing solution, achieving uniform dyeing, and is particularly suitable for scenarios with high requirements for dyeing uniformity, such as dyeing of dark cellulose fibers. The selection of the alkali agent slow-release agent in the present application is not particularly limited, and conventional alkali agent slow-release agents in the art can be used. In some embodiments, the alkali agent slow-release agent can be at least one of AIO541, AIO533, and AIO500, and the above alkali agent slow-release agents are all products from Qingyuan Enke Material Technology Co., Ltd.
[0027] The cellulose fiber of the present application is a type of fiber processed from natural cellulose, including natural cellulose fiber and regenerated cellulose fiber, wherein the natural cellulose fiber includes cotton fiber and hemp fiber, and the regenerated cellulose fiber includes viscose fiber, lyocell fiber, modal fiber, etc.
[0028] The pretreatment of the present application is different pretreatment before dyeing according to the type of cellulose fiber, for example, the pretreatment of woven fabric includes desizing, scouring and bleaching, the pretreatment of knitted fabric includes scouring and bleaching, wherein desizing is to remove sizing on woven fabric, scouring is to remove natural impurities on fabric by using chemical and physical mechanical action, and bleaching is to remove natural pigment on fabric and give fabric necessary and stable whiteness. After pretreatment, the cellulose fiber can make the dye better adsorbed on the fiber, fully combined with the fiber, more uniform in color, and more bright and firm in color.
[0029] In step 2) of the microemulsion dyeing method, after the pretreated cellulose fibers are immersed in the microemulsion dyeing solution, the temperature is raised to 80-100℃ and maintained for 20-60 min, and then the temperature is lowered to below 50℃, and the dyeing of the cellulose fibers is completed. Because the water consumption of the microemulsion system is greatly reduced compared to the traditional process, in the above dyeing process, the bath ratio of the cellulose fibers to the microemulsion dyeing solution can be 1:15-25, preferably 1:18-22.
[0030] In step 2) of the microemulsion dyeing method, the heating rate can be 1-3℃ / min.
[0031] In step 2) of the microemulsion dyeing method, the cooling rate can be 3-5℃ / min.
[0032] The microemulsion dyeing method of the present application can also include post-treatment of the dyeing, and the specific operation can be to remove the residual liquid attached to the dyed material obtained after step 2), and then sequentially perform baking, soaping and drying, wherein the baking conditions include a temperature of 110-140℃ and a time of 10-20 min.
[0033] The organic solvent in the existing dyeing system is difficult to remove, and a large amount of washing liquid needs to be used for washing, which consumes a large amount of water. The organic solvent selected in the present application is cyclopentyl methyl ether, which can be volatilized at high temperature and removed after baking treatment, greatly reducing the amount of washing agent and the number of water washing. Due to the above characteristics of cyclopentyl methyl ether, the cyclopentyl methyl ether in the present application can be recycled and utilized, and the specific operation can be to mix the remaining microemulsion dyeing solution after dyeing, the gas volatilized by baking, the residual liquid squeezed and collected, and the wastewater after washing, and then stand for stratification, collect the cyclopentyl methyl ether hydrophobic solvent in the supernatant, and continue to use it as raw material for preparing the microemulsion dyeing solution.
[0034] The microemulsion dyeing method of the present application will be further illustrated by the following examples. The examples are implemented on the premise of the technical solutions of the present application, and detailed implementation modes and specific operation processes are given, but the protection scope of the present application is not limited to the following examples.
[0035] In the following examples, the experimental methods are conventional methods in the art unless otherwise specified. The experimental materials used in the following examples can be commercially available unless otherwise specified.
[0036] Example 1 A water dyebath of 10 mL containing 0.1 g (2% o.m.f) of the alkali builder slow release agent AIO541 (from QINGYUAN ENKE MATERIAL TECHNOLOGY CO., LTD.) and 0.15 g (3% o.m.f.) of the nicotinic acid type active orange TCR-D (purchased from WUJIANG TAOYUAN DYE LTD.) active dye was prepared, 45 mL of cyclopentyl methyl ether was added, the resulting mixture was added dropwise to cyclopentyl methyl ether to 100 mL, and stirred at room temperature at a speed of 13000 r / min, so that the aqueous solution containing the dye was uniformly dispersed in the cyclopentyl methyl ether hydrophobic solvent in the form of tiny droplets to form a microemulsion dyebath.
[0037] 5 g of cotton fabric after scouring and bleaching was immersed in the prepared microemulsion dyebath, heated to 90°C at a rate of 2°C / min, and kept for 30 min, then cooled to 30°C at a rate of 4°C / min, the dyed cotton fabric was taken out, the dyebath remaining on the cotton fabric was squeezed out, and mixed with the microemulsion dyebath remaining after dyeing to obtain residual dyebath. After adding 20 mL of water to the residual dyebath and standing for stratification, water was added to the lower layer of the stratified residual dyebath to make all the residual dyebath reach 50 mL, the lower layer of the aqueous dye solution was taken out, its absorbance was detected, then its exhaustion rate was calculated and recorded in Table 1.
[0038] The dyed cotton fabric was baked at 120°C for 10 min, the cyclopentyl methyl ether hydrophobic solvent and water volatilized from the cotton fabric were removed, and finally the fabric was soaped and dried, the color depth (K / S value) of the dyed fabric was detected and recorded in Table 1.
[0039] The cyclopentyl methyl ether hydrophobic solvent in the remaining microemulsion system, baking volatilization and wastewater after washing was mixed and allowed to stand for stratification, the cyclopentyl methyl ether hydrophobic solvent in the supernatant was recovered and used as microemulsion raw material.
[0040] Example 2 A water dyebath of 10 mL containing 0.05 g (1% o.m.f) of the alkali builder slow release agent AIO533 (from QINGYUAN ENKE MATERIAL TECHNOLOGY CO., LTD.) and 0.05 g (1% o.m.f.) of the nicotinic acid type active orange TCR-5R (purchased from WUJIANG TAOYUAN DYE LTD.) active dye was prepared, 45 mL of cyclopentyl methyl ether was added, the resulting mixture was added dropwise to cyclopentyl methyl ether to 100 mL, and stirred at room temperature at a speed of 12000 r / min, so that the aqueous solution containing the dye was uniformly dispersed in the cyclopentyl methyl ether hydrophobic solvent in the form of tiny droplets to form a microemulsion dyebath.
[0041] Take the scoured and bleached cotton fabric 5g, immersed in the prepared microemulsion, with the rate of 1 ℃ / min to 80 ℃, after 60 min, then with the rate of 3 ℃ / min to 40 ℃, take out the dyed cotton fabric, squeeze the dye solution remaining on the cotton fabric, and mix with the residual microemulsion after dyeing, get the residual dyeing solution. After adding 20 mL of water to the residual dyeing solution, it is layered, then add water to the lower layer of the layered residual dyeing solution until all the residual dyeing solution reaches 100 mL, take the lower layer of the dye aqueous solution, detect its absorbance, then calculate its exhaustion rate and record in Table 1.
[0042] The dyed cotton fabric is baked at 120 ℃ for 10 min, the cyclopentyl methyl ether hydrophobic solvent adhered to the cotton fabric is volatilized, and finally it is soaped, dried, and the color depth (K / S value) of the dyed fabric is detected and recorded in Table 1.
[0043] The cyclopentyl methyl ether hydrophobic solvent in the residual microemulsion system, baking volatilization and wastewater after washing is mixed and layered, the cyclopentyl methyl ether hydrophobic solvent in the supernatant is recovered and used as microemulsion raw material.
[0044] Example 3 Prepare 10 mL of water dyeing solution containing 0.2 g (4% o.m.f) of alkali agent slow-release agent AIO500 (from Qingyuan Enke Material Technology Co., Ltd.) and 0.25 g (5% o.m.f.) of nicotinic acid type active red TCR-D (purchased from Wujiang Taoyuan Dyeing Co., Ltd.) active dye, then add 54 mL of cyclopentyl methyl ether, drop the obtained mixture into cyclopentyl methyl ether to 100 mL, and stir at room temperature at a speed of 8000 r / min, so that the dye-containing aqueous solution is uniformly dispersed in the cyclopentyl methyl ether hydrophobic solvent in the form of tiny droplets to form a microemulsion dyeing solution.
[0045] Take the scoured and bleached cotton fabric 5g, immersed in the prepared microemulsion, with the rate of 1 ℃ / min to 80 ℃, after 60 min, then with the rate of 3 ℃ / min to 40 ℃, take out the dyed cotton fabric, squeeze the dye solution remaining on the cotton fabric, and mix with the residual microemulsion after dyeing, get the residual dyeing solution. After adding 20 mL of water to the residual dyeing solution, it is layered, then add water to the lower layer of the layered residual dyeing solution until all the residual dyeing solution reaches 100 mL, take the lower layer of the dye aqueous solution, detect its absorbance, then calculate its exhaustion rate and record in Table 1.
[0046] The dyed cotton fabric is baked at 120 ℃ for 10 min, the cyclopentyl methyl ether hydrophobic solvent adhered to the cotton fabric is volatilized, and finally it is soaped, dried, and the color depth (K / S value) of the dyed fabric is detected and recorded in Table 1.
[0047] The remaining microemulsion system, baked volatiles and the cyclopentyl methyl ether hydrophobic solvent in the effluent wastewater from the microemulsion system are mixed and allowed to separate into layers. The cyclopentyl methyl ether hydrophobic solvent in the supernatant is recovered and used as the microemulsion feedstock.
[0048] Example 4 The difference from Example 1 is that 7 mL of an aqueous dye liquor containing 0.1 g (2% o.m.f) of the alkaline agent slow release agent AIO541 and 0.15 g (3% o.m.f.) of the nicotinic acid type reactive orange TCR-D reactive dye is prepared.
[0049] Example 5 The difference from Example 1 is that 8 mL of an aqueous dye liquor containing 0.1 g (2% o.m.f) of the alkaline agent slow release agent AIO541 and 0.15 g (3% o.m.f.) of the nicotinic acid type reactive orange TCR-D reactive dye is prepared.
[0050] Example 6 The difference from Example 1 is that 9 mL of an aqueous dye liquor containing 0.1 g (2% o.m.f) of the alkaline agent slow release agent AIO541 and 0.15 g (3% o.m.f.) of the nicotinic acid type reactive orange TCR-D reactive dye is prepared.
[0051] Example 7 The difference from Example 1 is that 11 mL of an aqueous dye liquor containing 0.1 g (2% o.m.f) of the alkaline agent slow release agent AIO541 and 0.15 g (3% o.m.f.) of the nicotinic acid type reactive orange TCR-D reactive dye is prepared.
[0052] Example 8 The difference from Example 1 is that 12 mL of an aqueous dye liquor containing 0.1 g (2% o.m.f) of the alkaline agent slow release agent AIO541 and 0.15 g (3% o.m.f.) of the nicotinic acid type reactive orange TCR-D reactive dye is prepared.
[0053] Example 9 The difference from Example 1 is that 10 mL of an aqueous dye liquor containing 0.05 g (1% o.m.f) of the solid alkaline slow release agent AIO541 and 0.15 g (3% o.m.f.) of the nicotinic acid type reactive orange TCR-D reactive dye is prepared.
[0054] Example 10 The difference from Example 1 is that 10 mL of an aqueous dye liquor containing 0.075 g (1.5% o.m.f) of the solid alkaline slow release agent AIO541 and 0.15 g (3% o.m.f.) of the nicotinic acid type reactive orange TCR-D reactive dye is prepared.
[0055] Example 11 The difference from Example 1 is that 10 mL of aqueous dye liquor containing 0.125 g (2.5% o.m.f.) of solid alkali slow-release agent AIO541 and containing 0.15 g (3% o.m.f.) of nicotinic acid type active orange TCR-D reactive dye is prepared.
[0056] Example 12 The difference from Example 1 is that 10 mL of aqueous dye liquor containing 0.15 g (3% o.m.f.) of solid alkali slow-release agent AIO541 and containing 0.15 g (3% o.m.f.) of nicotinic acid type active orange TCR-D reactive dye is prepared.
[0057] Example 13 The difference from Example 1 is that 10 mL of aqueous dye liquor containing 0.2 g (4% o.m.f.) of solid alkali slow-release agent AIO541 and containing 0.15 g (3% o.m.f.) of nicotinic acid type active orange TCR-D reactive dye is prepared.
[0058] Comparative Example 1 10 mL of aqueous dye liquor containing 0.15 g (3% o.m.f.) of nicotinic acid type active orange TCR-D (purchased from Wujiang Taoyuan Dyeing Co., Ltd.) reactive dye is prepared, 45 mL of cyclopentyl methyl ether is added, the mixture is added dropwise into cyclopentyl methyl ether to 100 mL, and the mixture is stirred at room temperature at a speed of 13000 r / min, so that the aqueous solution containing the dye is uniformly dispersed in the cyclopentyl methyl ether hydrophobic solvent in the form of tiny droplets to form a microemulsion dye liquor.
[0059] 5 g of cotton fabric after scouring and bleaching is immersed in the prepared microemulsion dye liquor, and after being heated to 90°C at a rate of 2°C / min, 0.1 g (2% o.m.f.) of alkali agent slow-release agent AIO541 (from Qingyuan Enke Material Technology Co., Ltd.) is added into the dyeing liquor, and the temperature is kept for 30 min, and then the temperature is lowered to 30°C at a rate of 4°C / min, the dyed cotton fabric is taken out, the dye liquor remaining on the cotton fabric is squeezed out, and mixed with the residual microemulsion dye liquor after dyeing, to obtain residual dye liquor. After 20 mL of water is added to the residual dye liquor and allowed to stand for stratification, water is added to the lower layer of the stratified dye aqueous solution to make all the residual dye liquor reach 50 mL, the lower layer of the dye aqueous solution is taken out, the absorbance is detected, and then the exhaustion rate is calculated and recorded in Table 1.
[0060] The dyed cotton fabric is baked at 120°C for 10 min, and the cyclopentyl methyl ether hydrophobic solvent and water adhering to the cotton fabric are volatilized, and finally the fabric is soaped and dried, and the color depth (K / S value) of the dyed fabric is detected and recorded in Table 1.
[0061] The remaining microemulsion system, baking volatile and washing wastewater of cyclopentyl methyl ether hydrophobic solvent mixture after standing stratification, recovery of cyclopentyl methyl ether hydrophobic solvent in the upper clear liquid, it can be used as microemulsion raw material continues to use.
[0062] Comparative Example 2 The difference from Example 1 is that the base agent slow-release agent AIO541 is replaced by sodium hydroxide base agent.
[0063] Comparative Example 3 The difference from Example 1 is that the base agent slow-release agent AIO541 is replaced by sodium carbonate base agent.
[0064] Comparative Example 4 The difference from Example 1 is that the water dyeing solution 15 mL containing 0.1 g (2% o.m.f.) of base agent slow-release agent AIO541 (from Qingyuan Enke Material Technology Co., Ltd.) and containing 0.15 g (3% o.m.f.) of nicotinic acid type active orange TCR-D (purchased from Wujiang Taoyuan Dyeing Co., Ltd.) active dye is configured.
[0065] Comparative Example 5 The difference from Example 1 is that 5 g of cotton fabric after scouring and bleaching is immersed in the prepared microemulsion dyeing solution, and after heating to 50°C, it is kept for 30 min.
[0066] Comparative Example 6 The difference from Example 1 is that 5 g of cotton fabric after scouring and bleaching is immersed in the prepared microemulsion dyeing solution, and after heating to 60°C, it is kept for 30 min.
[0067] Comparative Example 7 The difference from Example 1 is that 5 g of cotton fabric after scouring and bleaching is immersed in the prepared microemulsion dyeing solution, and after heating to 70°C, it is kept for 30 min.
[0068] Comparative Example 8 The water dyeing solution 100 mL containing 0.1 g (2% o.m.f.) of base agent slow-release agent AIO541 (from Qingyuan Enke Material Technology Co., Ltd.) and containing 0.15 g (3% o.m.f.) of nicotinic acid type active orange TCR-D (purchased from Wujiang Taoyuan Dyeing Co., Ltd.) active dye is configured.
[0069] 5 g of cotton fabric after scouring and bleaching is immersed in the prepared water dyeing solution, and after heating to 90°C at a rate of 2°C / min, it is kept for 30 min, and then it is cooled to 30°C at a rate of 4°C / min, the dyed cotton fabric is taken out, and the residual dyeing solution on the cotton fabric is squeezed out. The dyeing residual liquid is taken, and its absorbance is detected, and then its exhaustion rate is calculated and recorded in Table 1.
[0070] The dyed cotton fabric is baked at 120℃ for 10 minutes, and finally soaped, dried, and the color depth (K / S value) of the dyed fabric is detected and recorded in Table 1.
[0071] The dyeing rates of the fabrics in Examples 1-13 and Comparative Examples 1-8 are calculated, and the color depth (K / S value) of each dyed fabric is detected and recorded in Table 1.
[0072] Table 1
[0073] As can be seen from the results of Examples 1-20 in Table 1, effective dyeing of cotton fabric can be achieved by using the microemulsion dyeing method of the present application, and the dyeing rate can reach more than 90%, and at the same time, due to the high utilization rate of dyes, the amount of wastewater is reduced, and clean dyeing of cotton fabric is also achieved.
[0074] The above describes the preferred embodiments of the present application, but the present application is not limited thereto. Within the technical concept of the present application, various simple modifications can be made to the technical solutions of the present application, including the combination of various technical features in any other suitable manner, and these simple modifications and combinations should also be considered as disclosed by the present application, and all fall within the protection scope of the present application.
Claims
1. A microemulsion dyeing method, characterized in that: The method includes: 1) mixing a dye solution containing a reactive dye with an alkaline slow-release agent, and then mixing with a portion of cyclopentyl methyl ether, and then adding the resulting mixture dropwise to the remaining portion of cyclopentyl methyl ether to form a microemulsion dye solution, wherein the water content of the microemulsion dye solution is 7-12 vol.%, based on the total amount of cyclopentyl methyl ether used, the amount of the portion of cyclopentyl methyl ether used accounts for 50-60 vol.%, and the amount of the remaining portion of cyclopentyl methyl ether accounts for 40-50 vol.%; 2) Immersing the pretreated cellulose fibers in the microemulsion dye solution, heating to 80-100° C. and keeping the temperature for 20-60 minutes, and then cooling to below 50° C.
2. The method according to claim 1, characterized in that The water content of the microemulsion dye solution is 9-11 vol.%.
3. The method according to claim 1 or 2, characterized in that Based on the total amount of cyclopentyl methyl ether, the amount of the part of cyclopentyl methyl ether used is 52-56 vol.%, and the amount of the remaining part of cyclopentyl methyl ether used is 44-48 vol.%.
4. The method according to any one of claims 1 to 3, characterized in that In the microemulsion dye solution, the amount of the reactive dye is 1-5% (owf), the amount of the alkaline sustained-release agent is 1-4% (owf), and the content of the cyclopentyl methyl ether is 88-93 vol.%.
5. The method according to any one of claims 1 to 4, characterized in that The reactive dye is at least one of nicotinic acid reactive orange TCR-D, nicotinic acid reactive orange TCR-5R and nicotinic acid reactive red TCR-D.
6. The method according to any one of claims 1 to 5, characterized in that The alkaline sustained-release agent is at least one of AIO541, AIO533 and AIO500.
7. The method according to any one of claims 1 to 6, characterized in that In step 2), the bath ratio of the cellulose fiber to the microemulsion dye solution is 1:15-25.
8. The method according to any one of claims 1 to 7, characterized in that In step 2), the heating rate is 1-3°C / min.
9. The method according to any one of claims 1 to 8, characterized in that In step 2), the cooling rate is 3-5°C / min.
10. The method according to any one of claims 1 to 9, characterized in that The method further comprises: sequentially baking, soaping and drying the dyed material obtained after the treatment in step 2), wherein the baking conditions include: a temperature of 110-140° C. and a time of 10-20 minutes.