CN108951226B - Anhydrous dyeing medium based on ionic liquid, anhydrous dyeing method and dyeing medium recycling method - Google Patents
Anhydrous dyeing medium based on ionic liquid, anhydrous dyeing method and dyeing medium recycling method Download PDFInfo
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- CN108951226B CN108951226B CN201810864850.4A CN201810864850A CN108951226B CN 108951226 B CN108951226 B CN 108951226B CN 201810864850 A CN201810864850 A CN 201810864850A CN 108951226 B CN108951226 B CN 108951226B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/90—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using dyes dissolved in organic solvents or aqueous emulsions thereof
- D06P1/92—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using dyes dissolved in organic solvents or aqueous emulsions thereof in organic solvents
Abstract
The invention discloses an anhydrous dyeing medium based on ionic liquid and dyeing using the sameA method for the waterless dyeing of a medium and a method for the recovery of the dyeing medium. The dyeing medium contains 1-alkyl-3-methylimidazolium hydrogen sulfate [ Cnmim]HSO4And 1-alkyl-3-methylimidazolium tetrafluoroborate [ C ]nmim]BF4. The anhydrous dyeing method only uses the anhydrous dyeing medium based on the ionic liquid, does not need to add chemical raw materials such as acid, salt, surfactant and the like, and can realize the dyeing of materials such as acrylic fiber, wool, cotton and the like at a certain temperature. After the dyeing medium after dyeing is supplemented with part of dyes, the anhydrous dyeing medium based on the ionic liquid can be recycled for dyeing of the same dye. The residual dye can be separated out by mixing the dyeing medium after dyeing with carbon tetrachloride, and the dyeing medium can be recycled and used in the dyeing process equivalent to a fresh dyeing medium. The invention realizes waterless dyeing and solves the problem that a large amount of waste water and waste gas are generated in the traditional dyeing process to pollute the environment.
Description
Technical Field
The invention relates to the textile printing and dyeing industry, in particular to an anhydrous dyeing medium based on ionic liquid, an anhydrous dyeing method using the anhydrous dyeing medium and a recovery method of the anhydrous dyeing medium.
Background
Dyeing in the textile industry, also known as printing, dyeing or dyeing and finishing, is the dyeing of natural fibers or chemical fibers, and yarns, fabrics, garments and other articles made of the fibers. Textile printing and dyeing become indispensable important industries in modern society, and fully meet the requirements of people on the color diversity of daily clothes.
The textile printing and dyeing industry is typically a high energy consumption, high water consumption and high pollution industry. The dyeing wastewater contains substances such as sizing agent, dye, auxiliary agent, surfactant and the like, has complex components, has COD (chemical oxygen demand) of 1000mg/L on average, and has darker chroma due to the residual dye. The annual discharge amount of the textile printing and dyeing wastewater is about 20-23 million tons, which accounts for about 11% of national wastewater discharge, and the discharge amount of Chemical Oxygen Demand (COD) is about 24-30 million tons every year. The dyeing and finishing wastewater pollutants mainly come from fiber materials, textile sizing agents, dyes used for dyeing and finishing, chemical agents and the like, typical high-grade fabric dyeing and finishing wastewater mainly comprises desizing, scouring and bleaching wastewater, dyeing wastewater, mercerizing wastewater, after-finishing wastewater, equipment washing water and the like, and the pH value of the dyeing and finishing wastewater is higher and is usually between 10 and 11. In general, the printing and dyeing wastewater has the characteristics of high pollutant concentration, multiple types, high alkalinity, high toxicity, high chromaticity and the like, and belongs to one of the industrial wastewater which is difficult to treat.
In addition, the printing and dyeing waste gas is also remarkably discharged, and the printing and dyeing waste gas mainly contains substances such as formaldehyde, ammonia gas, polyphenyl and dye molecules and is discharged in the form of a high-temperature gas (120-170 ℃) mixture, and the main source of the high-temperature gas is a high-temperature setting machine.
In summary, the dyeing method adopted in the current printing and dyeing industry has the problems of large water consumption, large wastewater discharge amount, difficult treatment and large waste gas discharge amount. Therefore, there is an urgent need to find an anhydrous dyeing medium that can be recycled in the dyeing process and to develop a corresponding anhydrous dyeing method without wastewater and exhaust emission.
Disclosure of Invention
In order to solve the problems in the traditional printing and dyeing industry, the invention provides an anhydrous dyeing medium based on ionic liquid.
The anhydrous dyeing medium based on ionic liquid contains 1-alkyl-3-methylimidazolium hydrogen sulfate [ Cnmim]HSO4And 1-alkyl-3-methylimidazolium tetrafluoroborate [ C ]nmim]BF4。
The alkyl group comprises ethyl, butyl or octyl; further, the ethyl group, the butyl group or the octyl group means an ethyl group, an n-butyl group or an n-octyl group, respectively.
The ionic liquid is prepared by adopting a two-step method. With 1-butyl-3-methylimidazolium hydrogen sulfate [ Bmim ]]HSO4For example, N-methylimidazole and N-butyl bromide are first reacted under heating and stirring to produce brominated 1-butyl-3-methylimidazole [ Bmim ]]Br; the resulting brominated 1-butyl-3-methylimidazole [ Bmim ] is then reacted with a base]Br and cyclohexane are mixed, concentrated sulfuric acid is dripped in to generate 1-butyl-3-methylimidazole hydrogen sulfate [ Bmim]HSO4(ii) a Finally, the generated hydrogen bromide, normal hexane and other unreacted reactants are evaporated by using a rotary evaporator to obtain pure 1-butyl-3-methylimidazolium hydrogen sulfate [ Bmim ]]HSO4An ionic liquid.
The ionic liquid 1-alkyl-3-methylimidazolium hydrogen sulfate [ Cnmim]HSO4And 1-alkyl-3-methylimidazolium tetrafluoroborate [ C ]nmim]BF4All show a certain acidity, 1-alkyl-3-methylimidazolium hydrogen sulfate [ Cnmim]HSO4Has a pH of 1 to 2, 1-alkyl-3-methylimidazolium tetrafluoroborate [ C ]nmim]BF4The pH value of (A) is about 6.
The anhydrous dyeing medium based on ionic liquid contains ionic liquid 1-alkyl-3-methylimidazolium hydrogen sulfate [ Cnmim]HSO4And 1-alkyl-3-methylimidazolium tetrafluoroborate [ C ]nmim]BF4. By adjusting the proportion of the two ionic liquids, the anhydrous dyeing medium with different pH values based on the ionic liquid is obtained. For example, in order to obtain an anhydrous dyeing medium based on an ionic liquid with a pH of 4 to 5, 1-alkyl-3-methylimidazolium tetrafluoroborate [ C ]nmim]BF4Adding proper amount of 1-alkyl-3-methylimidazole hydrogen sulfate [ Cnmim]HSO4And (4) finishing.
In the anhydrous dyeing medium based on the ionic liquid, the ionic liquid can simultaneously play the roles of an acid-base regulator, salt, a leveling agent and water in the traditional dyeing process, so that the anhydrous dyeing medium can be used as an acid-free, salt-free, other-assistant-free and anhydrous dyeing medium.
In order to solve the problems existing in the traditional printing and dyeing industry, the invention also provides an anhydrous dyeing method, which comprises the following steps:
1) preparation of a dyeing medium: using 1-alkyl-3-methylimidazolium hydrogen sulfate [ C ]nmim]HSO4And 1-alkyl-3-methylimidazolium tetrafluoroborate [ C ]nmim]BF4Preparing an anhydrous dyeing medium based on an ionic liquid;
2) soaking: raising the temperature of the anhydrous dyeing medium based on the ionic liquid obtained in the step 1) to 60-95 ℃, putting the material to be dyed into the anhydrous dyeing medium, and soaking for 1-20 min;
3) dyeing: dyeing: putting a dye into the dyeing medium containing the materials in the step 2), uniformly stirring, keeping the temperature at 60-95 ℃ for 5-20 min, raising the temperature to be above 100 ℃, keeping the temperature for 10-60 min, and dyeing the materials;
4) cooling: reducing the temperature of the dyeing medium of step 3) to below 60 ℃;
5) and (3) post-treatment: taking out the dyed material obtained in the step 4), extruding the carried dyeing medium in an extrusion mode, washing the material and drying.
The anhydrous dyeing method, the material to be dyed in step 2) comprises acrylic fibers, wool and cotton, including but not limited to acrylic fibers, wool, cotton fibers, acrylic fabrics, wool fabrics, cotton fabrics, acrylic garments, wool garments and cotton clothes.
In the anhydrous dyeing method, the bath ratio ranges from 2 to 100:1, the bath ratio is also called as a liquid ratio and refers to the mass ratio of a dyeing medium to a material to be dyed, for example, when 1000 kg of the dyeing medium is used for 100 kg of textiles, the bath ratio is called as 10: 1.
Further preferably, the bath ratio of the anhydrous dyeing method is in the range of 5-50: 1.
In the anhydrous dyeing method, the preferable temperature of the dyeing medium in the soaking in the step 2) is 80-90 ℃, and the further preferable temperature is 85 ℃.
In the anhydrous dyeing method, the soaking time in the step 2) is 5-15 min, and the further preferred temperature is 10 min.
The dye refers to a dye that is soluble in the ionic liquid-based anhydrous dyeing medium, including but not limited to the dyes described below, including cationic dyes, acid dyes, and reactive dyes.
The cationic dye comprises cationic brilliant red, cationic pink, cationic brilliant blue, cationic yellow and the like.
The acid dye comprises acid brilliant blue, acid scarlet, acid golden yellow, acid orange and the like.
The reactive dye comprises reactive blue, reactive yellow, reactive black and the like.
The amount of the dye to be added depends on factors such as bath ratio and required dyeing depth, for example, if the approximate dyeing effect is to be achieved (the K/S value is about 10), 2% of the weight of the material to be dyed is required to be added when the bath ratio is 10:1, and 10% of the weight of the material to be dyed is required to be added when the bath ratio is 50: 1.
The K/S value is a parameter for representing dyeing effect, and the larger the value is, the better the dyeing effect is.
The form of the addition of the dye to the anhydrous ionic liquid-based dyeing medium may be the solid dye itself, e.g. a powder dye; it is also possible to dissolve the dye in an anhydrous dyeing medium based in part on an ionic liquid to form a dye liquor and add it to the dyeing medium.
In the anhydrous dyeing method, the temperature of the dyeing medium in the step 3) is 80-90 ℃ before the temperature is increased, and the further optimized temperature is 85 ℃.
According to the anhydrous dyeing method, the dyeing time before the temperature of the dyeing medium in the step 3) is increased is 5-20 min, and the further preferable temperature is 10 min.
In the anhydrous dyeing method, the temperature in the step 3) is uniformly increased, and the temperature increasing rate is 0.5-3 ℃/min. Further preferably, the temperature rise rate is 0.5 ℃/min to 1.5 ℃/min. A further preferred temperature rise rate is 1.0 deg.C/min.
In the anhydrous dyeing method, the temperature of the dyeing medium in the step 3) is increased to 100-120 ℃, and the further preferred temperature is 110 ℃.
According to the anhydrous dyeing method, the dyeing time after the temperature of the dyeing medium in the step 3) is increased is 20-40 min, and the further preferable temperature is 30 min.
In order to obtain better dyeing effect, the step 3) of the anhydrous dyeing method can be used for dyeing under the condition of intensive mixing, and the means of intensive mixing includes but is not limited to continuous stirring, stirring and the like.
The temperature of the dyeing medium in the step 4) of the anhydrous dyeing method is reduced to below 60 ℃. Further preferably, the temperature is reduced to 50 ℃ or lower.
In the anhydrous dyeing method, the temperature in the step 4) is reduced at a constant speed, and the temperature reduction rate is 0.5-5 ℃/min. Further preferably, the temperature decrease rate is 0.5 ℃/min to 2.5 ℃/min. A more preferable temperature lowering rate is 1.0 ℃/min to 2.0 ℃/min.
The anhydrous dyeing method, the material of step 5) which is dyed is washed by water. The washed water contains the anhydrous dyeing medium based on the ionic liquid and the dye, and the separation of the water, the anhydrous dyeing medium based on the ionic liquid and the dye can be realized after the water is simply separated by a method of evaporating the water. The separated anhydrous dyeing medium and dye based on the ionic liquid can be reused in the step 3) of the anhydrous dyeing method, and the separated water can be reused in the step 5) of the anhydrous dyeing method.
The anhydrous dyeing method, namely the anhydrous dyeing medium based on the ionic liquid after the dyeing in the step 5) is finished can be recycled. And (3) part of dye is remained in the anhydrous dyeing medium based on the ionic liquid after dyeing is finished, when multiple batches of dyeing are repeatedly carried out, the dye is directly supplemented into the anhydrous dyeing medium, and a proper amount of material to be dyed is added, so that the next batch of dyeing operation can be carried out.
In order to solve the problem of recycling the anhydrous dyeing medium based on the ionic liquid, the invention also provides a method for recovering the anhydrous dyeing medium based on the ionic liquid, which comprises the following steps: firstly, mixing a dyeing medium containing residual dye with carbon tetrachloride after dyeing is finished, wherein the dyeing medium and the carbon tetrachloride are mutually soluble, and the dye is separated out in a solid form; then carrying out solid-liquid separation to obtain liquid containing a dyeing medium and carbon tetrachloride and dye solid; and finally evaporating carbon tetrachloride in the liquid containing the dyeing medium and the carbon tetrachloride to obtain the dyeing medium.
After carbon tetrachloride is added to the used anhydrous-based dyeing medium, the ionic liquid is mutually soluble with the carbon tetrachloride, and the residual dye is settled at the bottom in a solid form.
According to the method for recovering the anhydrous dyeing medium based on the ionic liquid, the volume ratio of the dyeing medium containing the residual dye to carbon tetrachloride after dyeing is 2:1 to 1: 2.
The method for recovering the anhydrous dyeing medium based on the ionic liquid comprises the existing methods for separating the solid and the liquid, such as filtration, centrifugation, gravity settling and the like.
In the method for recovering the anhydrous dyeing medium based on the ionic liquid, the solid-liquid separation method is preferably a filtration method, for example, the adopted filtration medium is filter paper or a filter membrane, and the separation of the dye precipitation and the ionic liquid system is carried out by adopting a suction filtration mode.
The method for recycling the anhydrous dyeing medium based on the ionic liquid is used for separating the anhydrous dyeing medium based on the ionic liquid from carbon tetrachloride by utilizing the boiling point difference between the anhydrous dyeing medium based on the ionic liquid and the carbon tetrachloride, and means that the liquid is heated to a certain temperature, so that a substance with a low boiling point is gasified and leaves a liquid main body, and a substance with a high boiling point still exists in a liquid form, thereby realizing the separation of the two substances. The boiling point of carbon tetrachloride is 76.8 ℃, while the anhydrous dyeing medium based on ionic liquids consists essentially of 1-alkyl-3-methylimidazolium hydrogen sulfate [ C ]nmim]HSO4And 1-alkyl-3-methylimidazolium tetrafluoroborate [ C ]nmim]BF4The boiling point of the composition is higher than 300 ℃, the difference between the two is large, and therefore carbon tetrachloride can be evaporated at the temperature of below 300 ℃. The separation can be carried out by adopting methods such as distillation, rectification, rotary evaporation and the like.
With the method for recovering the anhydrous dyeing medium based on the ionic liquid, more than 70% of the dye can be removed. The recovery operation may be performed a plurality of times for more complete removal of the remaining dye, for example, 3 times of recovery operation may achieve a dye removal rate of 98% or more.
The anhydrous dyeing medium based on the ionic liquid and with the dye removed, which is obtained by adopting the method for recovering the anhydrous dyeing medium based on the ionic liquid, can be used as a fresh dyeing medium and used for dyeing processes of different dyes.
The dye obtained by the method for recovering the anhydrous dyeing medium based on the ionic liquid can be used for dyeing processes of other batches of the same dye.
The carbon tetrachloride obtained by the method for recovering the anhydrous dyeing medium based on the ionic liquid can be used for the recovery process of other batches of the anhydrous dyeing medium based on the ionic liquid containing residual dye.
The anhydrous dyeing medium based on the ionic liquid, the anhydrous dyeing method and the recovery method of the anhydrous dyeing medium based on the ionic liquid, provided by the invention, overcome the defects of high energy consumption, high water consumption and high pollution of the existing dyeing and finishing process, and can provide a better technical scheme for energy conservation and emission reduction in the dyeing and finishing industry.
Effects of the invention
The anhydrous dyeing medium based on the ionic liquid, the anhydrous dyeing method and the recovery method of the anhydrous dyeing medium based on the ionic liquid have the advantages that: firstly, an anhydrous dyeing process is realized, and the washing water after dyeing can be recovered or recycled by adopting a proper method, so that the water consumption in the dyeing process is greatly reduced; secondly, chemical raw materials such as acid, salt and leveling auxiliary agent are not required to be added in the dyeing process, so that the consumption of the dyeing process is greatly reduced; no waste water and waste gas are generated, and the pollution to the environment is avoided; and fourthly, the dyeing medium and the dye are recycled.
Detailed Description
Example 1
Weighing ionic liquid [ Bmim ]]BF4(1-butyl-3-methylimidazolium tetrafluoroborate) 1500g in a container, and under the stirring condition, dropwise adding an ionic liquid [ Bmim [ ]]HSO4(1-butyl-3-methylimidazolium hydrogen sulfate), and measuring pH, and stopping adding ionic liquid [ Bmim ] when pH reaches 4.5]HSO4The preparation of an anhydrous dyeing medium based on an ionic liquid is completed by using [ Bmim ]]HSO4About 2 g.
Example 2
Weighing ionic liquid [ C ]2mim]BF4(1-Ethyl-3-methylimidazolium tetrafluoroborate) 2000g in a container, adding an ionic liquid [ C ] under stirring6mim]HSO4(1-octyl-3-methylimidazolium hydrogen sulfate), simultaneously measuring the pH value, and stopping adding the ionic liquid [ C ] when the pH value reaches 4.06mim]HSO4The preparation of an anhydrous dyeing medium based on ionic liquids is carried out using [ C ]6mim]HSO4About 4 g.
Example 3
Weighing ionic liquid [ C ]6mim]BF49000g of (1-octyl-3-methylimidazolium tetrafluoroborate) was placed in a vessel, and an ionic liquid [ C ] was added thereto with stirring2mim]HSO4(1-ethyl-3-methylimidazolium hydrogen sulfate), simultaneously measuring the pH value, and stopping adding the ionic liquid [ C ] when the pH value reaches 5.02mim]HSO4The preparation of an anhydrous dyeing medium based on ionic liquids is carried out using [ C ]2mim]HSO4About 1.5 g.
The anhydrous dyeing medium based on the ionic liquid, which is described in examples 1 to 3, is used in the dyeing process without adding water or adding chemical agents such as acid-base regulator, salt, leveling agent and the like, so that the anhydrous dyeing medium can be used as an acid-free, salt-free, other-aid and anhydrous dyeing medium.
Example 4
The specific operation steps of using the anhydrous dyeing medium based on the ionic liquid to carry out anhydrous dyeing are as follows:
1) preparation of a dyeing medium: an anhydrous ionic liquid-based dyeing medium, 15g, was prepared as described in example 1;
2) soaking: raising the temperature of the anhydrous dyeing medium based on the ionic liquid obtained in the step 1) to 85 ℃, putting the acrylic fiber into the anhydrous dyeing medium at a bath ratio of 50:1, and soaking for 10 min;
3) dyeing: weighing 0.03g of cationic brilliant red 5GN dye, putting into the anhydrous dyeing medium containing the material to be dyed in the step 2) and based on the ionic liquid, uniformly stirring, keeping the temperature at 85 ℃ for 15min, then increasing the temperature to 100 ℃ at the speed of 1 ℃/min, and keeping the temperature for 30 min;
4) cooling: reducing the temperature of the staining medium of step 3) to 50 ℃ at a rate of 2 ℃/min;
5) and (3) post-treatment: taking out the dyed material obtained in the step 4), extruding the carried dyeing medium by extrusion, washing the dyed material with water, and drying.
The dried dyed material was measured using a K/S colorimeter of UITRASCAN XE, a precision instruments manufacturing Co., Ltd., and the measured K/S value was 12.21, which is higher than 10.88 of the K/S value of the dyed material obtained by the conventional dyeing method under the equivalent conditions, indicating that the anhydrous dyeing method can obtain a better dyeing effect.
The washing water in the step 5) is separated from the anhydrous dyeing medium and the dye based on the ionic liquid by adopting a rotary evaporation method, the anhydrous dyeing medium and the dye based on the ionic liquid obtained after separation can be reused in the step 3) of the anhydrous dyeing method, the water obtained after separation can be reused for washing in the step 5) of the anhydrous dyeing method, and the water reuse rate is more than 98%.
Compared with the traditional dyeing method, the water consumption of the waterless dyeing method is reduced by more than 98%, chemical raw materials such as acid, salt and leveling auxiliary agent are not required to be added, the consumption is reduced by 100%, and the generation of waste water and waste gas is reduced by 100%.
Example 5
The specific operation steps of using the anhydrous dyeing medium based on the ionic liquid to carry out anhydrous dyeing are as follows:
1) preparation of a dyeing medium: 20g of an anhydrous ionic liquid-based dyeing medium was prepared as described in example 2;
2) soaking: raising the temperature of the anhydrous dyeing medium based on the ionic liquid obtained in the step 1) to 95 ℃, putting the wool fabric into the anhydrous dyeing medium at a bath ratio of 100:1, and soaking for 1 min;
3) dyeing: weighing 0.03G of acid brilliant blue G dye, dissolving the weighed acid brilliant blue G dye in 10G of the anhydrous dyeing medium based on the ionic liquid prepared in the step 1), pouring the weighed acid brilliant blue G dye into the anhydrous dyeing medium based on the ionic liquid containing the material to be dyed in the step 2), uniformly stirring the mixture, keeping the temperature at 95 ℃ for 5min, and then raising the temperature to 110 ℃ for 10 min;
4) cooling: reducing the temperature of the dyeing medium of step 3) to 70 ℃;
5) and (3) post-treatment: taking out the dyed material obtained in the step 4), extruding the carried dyeing medium by extrusion, washing the dyed material with water, and drying.
The dried dyed material was measured using a K/S colorimeter of UITRASCAN XE, a precision instruments manufacturing Co., Ltd., to obtain a K/S value of 12.11, and the conventional dyeing method was used to obtain a K/S value of 11.88 for the dyed material under the equivalent conditions, indicating that the anhydrous dyeing method can achieve a better dyeing effect.
And (3) separating water, the anhydrous dyeing medium based on the ionic liquid and the dye from the washing water obtained in the step 5) by adopting a reduced pressure distillation method, wherein the anhydrous dyeing medium based on the ionic liquid and the dye obtained after separation can be reused in the step 3) of the anhydrous dyeing method, the water obtained after separation can be reused for washing in the step 5) of the anhydrous dyeing method, and the water reuse rate is more than 98%.
Compared with the traditional dyeing method, the water consumption of the waterless dyeing method is reduced by more than 98%, chemical raw materials such as acid, salt and leveling auxiliary agent are not required to be added, the consumption is reduced by 100%, and the generation of waste water and waste gas is reduced by 100%.
Example 6
The specific operation steps of using the anhydrous dyeing medium based on the ionic liquid to carry out anhydrous dyeing are as follows:
1) preparation of a dyeing medium: an anhydrous ionic liquid-based dyeing medium, 15g, was prepared as described in example 3;
2) soaking: raising the temperature of the anhydrous dyeing medium based on the ionic liquid obtained in the step 1) to 60 ℃, putting the cotton fiber into the anhydrous dyeing medium at a bath ratio of 80:1, and soaking for 20 min;
3) dyeing: weighing 0.02g of active blue KNR dye, putting the active blue KNR dye into the anhydrous dyeing medium containing the material to be dyed in the step 2) and based on the ionic liquid, uniformly stirring, keeping the temperature at 60 ℃ for 30min, then increasing the temperature to 100 ℃ at the speed of 3 ℃/min, and keeping the temperature for 60 min;
4) cooling: reducing the temperature of the staining medium of step 3) to 40 ℃ at a rate of 5 ℃/min;
5) and (3) post-treatment: taking out the dyed material obtained in the step 4), extruding the carried dyeing medium by extrusion, washing the dyed material with water, and drying.
The dried dyed material was measured using a K/S colorimeter of UITRASCAN XE, a precision instruments manufacturing Co., Ltd., to obtain a K/S value of 10.06, and the conventional dyeing method was used to obtain a K/S value of 9.88 for the dyed material under the same conditions, indicating that the anhydrous dyeing method can achieve a better dyeing effect.
The washing water in the step 5) is separated from the anhydrous dyeing medium and the dye based on the ionic liquid by adopting a rotary evaporation method, the anhydrous dyeing medium and the dye based on the ionic liquid obtained after separation can be reused in the step 3) of the anhydrous dyeing method, the water obtained after separation can be reused for washing in the step 5) of the anhydrous dyeing method, and the water reuse rate is more than 98%.
Compared with the traditional dyeing method, the water consumption of the waterless dyeing method is reduced by more than 98%, chemical raw materials such as acid, salt and leveling auxiliary agent are not required to be added, the consumption is reduced by 100%, and the generation of waste water and waste gas is reduced by 100%.
Example 7
The specific operation steps of using the anhydrous dyeing medium based on the ionic liquid to carry out anhydrous dyeing are as follows:
1) preparation of a dyeing medium: 100g of an anhydrous ionic liquid-based dyeing medium was prepared as described in example 1;
2) soaking: raising the temperature of the anhydrous dyeing medium based on the ionic liquid obtained in the step 1) to 90 ℃, and putting the acrylic fiber into the anhydrous dyeing medium, wherein the bath ratio is 30: 1, soaking for 15 min;
3) dyeing: weighing 0.07g of cationic pink FG dye, adding into the anhydrous dyeing medium containing the material to be dyed in the step 2) based on the ionic liquid, uniformly stirring, keeping the temperature at 90 ℃ for 15min, then increasing the temperature to 110 ℃ at the speed of 1.5 ℃/min, and keeping the temperature for 40 min;
4) cooling: reducing the temperature of the staining medium of step 3) to 60 ℃ at a rate of 1 ℃/min;
5) and (3) post-treatment: taking out the dyed material obtained in the step 4), extruding the carried dyeing medium by extrusion, washing the dyed material with water, and drying.
The dried dyed material was measured using a K/S colorimeter of UITRASCAN XE, a precision instruments manufacturing Co., Ltd., to obtain a K/S value of 12.21, which is higher than 9.88, which is the K/S value of the dyed material obtained by the conventional dyeing method under the equivalent conditions, indicating that the anhydrous dyeing method can obtain a better dyeing effect.
And (3) separating water, the anhydrous dyeing medium based on the ionic liquid and the dye from the washing water obtained in the step 5) by adopting a distillation method, wherein the anhydrous dyeing medium based on the ionic liquid and the dye obtained after separation can be reused in the step 3) of the anhydrous dyeing method, the water obtained after separation can be reused for washing in the step 5) of the anhydrous dyeing method, and the water reuse rate is more than 98%.
Compared with the traditional dyeing method, the water consumption of the waterless dyeing method is reduced by more than 98%, chemical raw materials such as acid, salt and leveling auxiliary agent are not required to be added, the consumption is reduced by 100%, and the generation of waste water and waste gas is reduced by 100%.
Example 8
The specific operation steps of using the anhydrous dyeing medium based on the ionic liquid to carry out anhydrous dyeing are as follows:
1) preparation of a dyeing medium: 50g of an anhydrous ionic liquid-based dyeing medium was prepared as described in example 1;
2) soaking: raising the temperature of the anhydrous dyeing medium based on the ionic liquid obtained in the step 1) to 80 ℃, putting the acrylic fiber into the anhydrous dyeing medium at a bath ratio of 10:1, and soaking for 5 min;
3) dyeing: weighing 1.5g of cationic brilliant blue RL dye, adding into the anhydrous dyeing medium containing the material to be dyed in the step 2) based on the ionic liquid, uniformly stirring, keeping the temperature at 80 ℃ for 20min, then increasing the temperature to 130 ℃ at the speed of 0.5 ℃/min, and keeping the temperature for 20 min;
4) cooling: reducing the temperature of the staining medium of step 3) to 30 ℃ at a rate of 0.5 ℃/min;
5) and (3) post-treatment: taking out the dyed material obtained in the step 4), extruding the carried dyeing medium by extrusion, washing the dyed material with water, and drying.
The dried dyed material was measured using a K/S colorimeter of UITRASCAN XE, a precision instruments manufacturing Co., Ltd., and the measured K/S value was 11.62, which is higher than 9.88 of the K/S value of the dyed material obtained by the conventional dyeing method under the equivalent conditions, indicating that the anhydrous dyeing method can obtain a better dyeing effect.
And (3) separating water, the anhydrous dyeing medium based on the ionic liquid and the dye from the washing water obtained in the step 5) by adopting a reduced pressure distillation method, wherein the anhydrous dyeing medium based on the ionic liquid and the dye obtained after separation can be reused in the step 3) of the anhydrous dyeing method, the water obtained after separation can be reused for washing in the step 5) of the anhydrous dyeing method, and the water reuse rate is more than 98%.
Compared with the traditional dyeing method, the water consumption of the waterless dyeing method is reduced by more than 98%, chemical raw materials such as acid, salt and leveling auxiliary agent are not required to be added, the consumption is reduced by 100%, and the generation of waste water and waste gas is reduced by 100%.
Example 9
The specific operation steps of using the anhydrous dyeing medium based on the ionic liquid to carry out anhydrous dyeing are as follows:
1) preparation of a dyeing medium: 60g of an anhydrous ionic liquid-based dyeing medium was prepared as described in example 1;
2) soaking: raising the temperature of the anhydrous dyeing medium based on the ionic liquid obtained in the step 1) to 70 ℃, putting the acrylic fiber into the anhydrous dyeing medium at a bath ratio of 20:1, and soaking for 10 min;
3) dyeing: weighing 1.8g of cationic yellow X-GL dye, putting into the anhydrous dyeing medium containing the material to be dyed in the step 2) and based on the ionic liquid, uniformly stirring, keeping the temperature at 70 ℃ for 10min, then increasing the temperature to 110 ℃ at the speed of 1 ℃/min, and keeping the temperature for 20 min;
4) cooling: reducing the temperature of the staining medium of step 3) to 60 ℃ at a rate of 1 ℃/min;
5) and (3) post-treatment: taking out the dyed material obtained in the step 4), extruding the carried dyeing medium by extrusion, washing the dyed material with water, and drying.
The dried dyed material was measured using a K/S colorimeter of UITRASCAN XE, a precision instruments manufacturing Co., Ltd., and the measured K/S value was 11.82, which is higher than 9.91, which is the K/S value of the dyed material obtained by the conventional dyeing method under the equivalent conditions, indicating that the anhydrous dyeing method can obtain a better dyeing effect.
And (3) separating water, the anhydrous dyeing medium based on the ionic liquid and the dye from the washing water obtained in the step 5) by adopting a reduced pressure distillation method, wherein the anhydrous dyeing medium based on the ionic liquid and the dye obtained after separation can be reused in the step 3) of the anhydrous dyeing method, the water obtained after separation can be reused for washing in the step 5) of the anhydrous dyeing method, and the water reuse rate is more than 98%.
Compared with the traditional dyeing method, the water consumption of the waterless dyeing method is reduced by more than 98%, chemical raw materials such as acid, salt and leveling auxiliary agent are not required to be added, the consumption is reduced by 100%, and the generation of waste water and waste gas is reduced by 100%.
Example 10
The specific operation steps of using the anhydrous dyeing medium based on the ionic liquid to carry out anhydrous dyeing are as follows:
1) preparation of a dyeing medium: 20g of an anhydrous ionic liquid-based dyeing medium was prepared as described in example 1;
2) soaking: raising the temperature of the anhydrous dyeing medium based on the ionic liquid obtained in the step 1) to 85 ℃, putting the wool into the anhydrous dyeing medium, and soaking for 10min at a bath ratio of 50: 1;
3) dyeing: weighing 0.04g of acid scarlet GR dye, putting into the anhydrous dyeing medium containing the material to be dyed in the step 2) and based on the ionic liquid, uniformly stirring, keeping the temperature at 85 ℃ for 15min, then increasing the temperature to 100 ℃ at the speed of 1 ℃/min, and keeping the temperature for 30 min;
4) cooling: reducing the temperature of the staining medium of step 3) to 50 ℃ at a rate of 2 ℃/min;
5) and (3) post-treatment: taking out the dyed material obtained in the step 4), extruding the carried dyeing medium by extrusion, washing the dyed material with water, and drying.
The dried dyed material was measured using a K/S colorimeter of UITRASCAN XE, a precision instruments manufacturing Co., Ltd., and the measured K/S value was 12.81, which is higher than 11.96 of the K/S value of the dyed material obtained by the conventional dyeing method under the equivalent conditions, indicating that the anhydrous dyeing method can obtain a better dyeing effect.
The washing water in the step 5) is separated from the anhydrous dyeing medium and the dye based on the ionic liquid by adopting a rotary evaporation method, the anhydrous dyeing medium and the dye based on the ionic liquid obtained after separation can be reused in the step 3) of the anhydrous dyeing method, the water obtained after separation can be reused for washing in the step 5) of the anhydrous dyeing method, and the water reuse rate is more than 98%.
Compared with the traditional dyeing method, the water consumption of the waterless dyeing method is reduced by more than 98%, chemical raw materials such as acid, salt and leveling auxiliary agent are not required to be added, the consumption is reduced by 100%, and the generation of waste water and waste gas is reduced by 100%.
Example 11
The specific operation steps of using the anhydrous dyeing medium based on the ionic liquid to carry out anhydrous dyeing are as follows:
1) preparation of a dyeing medium: an anhydrous ionic liquid-based dyeing medium (30 g) was prepared as described in example 2;
2) soaking: raising the temperature of the anhydrous dyeing medium based on the ionic liquid obtained in the step 1) to 95 ℃, putting the wool fabric into the anhydrous dyeing medium at a bath ratio of 100:1, and soaking for 1 min;
3) dyeing: weighing 0.05G of acid golden yellow G dye, dissolving the acid golden yellow G dye in 10G of the anhydrous dyeing medium based on the ionic liquid prepared in the step 1), pouring the acid golden yellow G dye into the anhydrous dyeing medium based on the ionic liquid containing the material to be dyed in the step 2), uniformly stirring the mixture, keeping the temperature at 95 ℃ for 5min, and then raising the temperature to 110 ℃ for 10 min;
4) cooling: reducing the temperature of the dyeing medium of step 3) to 70 ℃;
5) and (3) post-treatment: taking out the dyed material obtained in the step 4), extruding the carried dyeing medium by extrusion, washing the dyed material with water, and drying.
The dried dyed material was measured using a K/S colorimeter of UITRASCAN XE, a precision instruments manufacturing Co., Ltd., to obtain a K/S value of 12.01, and the conventional dyeing method was used to obtain a dyed material having a K/S value of 10.78 under the same conditions, indicating that the anhydrous dyeing method can achieve a better dyeing effect.
And (3) separating water, the anhydrous dyeing medium based on the ionic liquid and the dye from the washing water obtained in the step 5) by adopting a reduced pressure distillation method, wherein the anhydrous dyeing medium based on the ionic liquid and the dye obtained after separation can be reused in the step 3) of the anhydrous dyeing method, the water obtained after separation can be reused for washing in the step 5) of the anhydrous dyeing method, and the water reuse rate is more than 98%.
Compared with the traditional dyeing method, the water consumption of the waterless dyeing method is reduced by more than 98%, chemical raw materials such as acid, salt and leveling auxiliary agent are not required to be added, the consumption is reduced by 100%, and the generation of waste water and waste gas is reduced by 100%.
Example 12
The specific operation steps of using the anhydrous dyeing medium based on the ionic liquid to carry out anhydrous dyeing are as follows:
1) preparation of a dyeing medium: an anhydrous ionic liquid-based dyeing medium, 15g, was prepared as described in example 3;
2) soaking: raising the temperature of the anhydrous dyeing medium based on the ionic liquid obtained in the step 1) to 60 ℃, putting the wool into the anhydrous dyeing medium, and soaking for 20min at a bath ratio of 80: 1;
3) dyeing: weighing 0.02g of acid orange dye, putting into the anhydrous dyeing medium containing the material to be dyed in the step 2) and based on the ionic liquid, uniformly stirring, keeping the temperature at 60 ℃ for 30min, then increasing the temperature to 100 ℃ at the speed of 3 ℃/min, and keeping the temperature for 60 min;
4) cooling: reducing the temperature of the staining medium of step 3) to 40 ℃ at a rate of 5 ℃/min;
5) and (3) post-treatment: taking out the dyed material obtained in the step 4), extruding the carried dyeing medium by extrusion, washing the dyed material with water, and drying.
The dried dyed material was measured using a K/S colorimeter of UITRASCAN XE, a precision instruments manufacturing Co., Ltd., to obtain a K/S value of 12.32, and the conventional dyeing method was used to obtain a K/S value of 11.98 for the dyed material under the equivalent conditions, indicating that the anhydrous dyeing method can achieve a better dyeing effect.
The washing water in the step 5) is separated from the anhydrous dyeing medium and the dye based on the ionic liquid by adopting a rotary evaporation method, the anhydrous dyeing medium and the dye based on the ionic liquid obtained after separation can be reused in the step 3) of the anhydrous dyeing method, the water obtained after separation can be reused for washing in the step 5) of the anhydrous dyeing method, and the water reuse rate is more than 98%.
Compared with the traditional dyeing method, the water consumption of the waterless dyeing method is reduced by more than 98%, chemical raw materials such as acid, salt and leveling auxiliary agent are not required to be added, the consumption is reduced by 100%, and the generation of waste water and waste gas is reduced by 100%.
Example 13
The specific operation steps of using the anhydrous dyeing medium based on the ionic liquid to carry out anhydrous dyeing are as follows:
1) preparation of a dyeing medium: 45g of an anhydrous ionic liquid-based dyeing medium was prepared as described in example 3;
2) soaking: raising the temperature of the anhydrous dyeing medium based on the ionic liquid obtained in the step 1) to 60 ℃, putting the cotton clothes into the anhydrous dyeing medium at a bath ratio of 80:1, and soaking for 20 min;
3) dyeing: weighing 0.06g of active black KN-B dye, putting into the anhydrous dyeing medium containing the material to be dyed in the step 2) and based on the ionic liquid, uniformly stirring, keeping the temperature at 60 ℃ for 30min, then increasing the temperature to 100 ℃ at the speed of 3 ℃/min, and keeping the temperature for 60 min;
4) cooling: reducing the temperature of the staining medium of step 3) to 40 ℃ at a rate of 5 ℃/min;
5) and (3) post-treatment: taking out the dyed material obtained in the step 4), extruding the carried dyeing medium by extrusion, washing the dyed material with water, and drying.
The dried dyed material was measured using a K/S colorimeter of UITRASCAN XE, a precision instruments manufacturing Co., Ltd., to obtain a K/S value of 11.06, and the conventional dyeing method was used to obtain a K/S value of 10.81 for the dyed material under the equivalent conditions, indicating that the anhydrous dyeing method can achieve a better dyeing effect.
The washing water in the step 5) is separated from the anhydrous dyeing medium and the dye based on the ionic liquid by adopting a rotary evaporation method, the anhydrous dyeing medium and the dye based on the ionic liquid obtained after separation can be reused in the step 3) of the anhydrous dyeing method, the water obtained after separation can be reused for washing in the step 5) of the anhydrous dyeing method, and the water reuse rate is more than 98%.
Compared with the traditional dyeing method, the water consumption of the waterless dyeing method is reduced by more than 98%, chemical raw materials such as acid, salt and leveling auxiliary agent are not required to be added, the consumption is reduced by 100%, and the generation of waste water and waste gas is reduced by 100%.
Example 14
The specific operation steps of using the anhydrous dyeing medium based on the ionic liquid to carry out anhydrous dyeing are as follows:
1) preparation of a dyeing medium: 200g of an anhydrous ionic liquid-based dyeing medium was prepared as described in example 1;
2) soaking: raising the temperature of the anhydrous dyeing medium based on the ionic liquid obtained in the step 1) to 85 ℃, putting the cotton fabric into the anhydrous dyeing medium at a bath ratio of 5:1, and soaking for 10 min;
3) dyeing: weighing 0.4g of reactive yellow 39 dye, putting the weighed reactive yellow 39 dye into the anhydrous dyeing medium containing the material to be dyed in the step 2) and based on the ionic liquid, uniformly stirring, keeping the temperature at 85 ℃ for 40min, then increasing the temperature to 100 ℃ at the speed of 1 ℃/min, and keeping the temperature for 30 min;
4) cooling: reducing the temperature of the staining medium of step 3) to 50 ℃ at a rate of 2 ℃/min;
5) and (3) post-treatment: taking out the dyed material obtained in the step 4), extruding the carried dyeing medium by extrusion, washing the dyed material with water, and drying.
Repeating the operation process for 7 times to respectively obtain 7 batches of dyed cotton fabrics. The dried dyed acrylic fibers were measured using a K/S colorimeter of UITRASCAN XE, a precision instruments manufacturing Co., Ltd., and the measured K/S values were 11.21, 10.31, 9.81, 8.42, 9.27, 10.53, 11.11, respectively, the average value was 10.09, and the variance was 0.89, indicating that the waterless dyeing method had good stability.
Example 15
The specific operation steps of using the anhydrous dyeing medium based on the ionic liquid to carry out anhydrous dyeing are as follows:
1) preparation of a dyeing medium: 200g of an anhydrous ionic liquid-based dyeing medium was prepared as described in example 1;
2) soaking: raising the temperature of the anhydrous dyeing medium based on the ionic liquid obtained in the step 1) to 85 ℃, putting the acrylic fiber into the anhydrous dyeing medium at a bath ratio of 5:1, and soaking for 10 min;
3) dyeing: weighing 0.4g of cationic brilliant red 5GN dye, putting into the anhydrous dyeing medium containing the material to be dyed in the step 2) based on the ionic liquid, uniformly stirring, keeping the temperature at 85 ℃ for 40min, then increasing the temperature to 100 ℃ at the speed of 1 ℃/min, and keeping the temperature for 30 min;
4) cooling: reducing the temperature of the staining medium of step 3) to 50 ℃ at a rate of 2 ℃/min;
5) and (3) post-treatment: taking out the dyed material obtained in the step 4), extruding the carried dyeing medium by extrusion, washing the dyed material with water, and drying.
Repeating the operation process for 7 times to respectively obtain 7 batches of dyed acrylic fibers. The dried dyed acrylic fibers were measured with a K/S colorimeter of UITRASCAN XE, a precision instruments manufacturing Co., Ltd., and the measured K/S values were 10.21, 10.31, 11.31, 12.42, 12.07, 11.33, 14.11, respectively, the average value was 11.68, and the variance was 1.56, indicating that the waterless dyeing method had better stability.
Example 16
The anhydrous ionic liquid-based staining medium recovered in step 5) of example 4 was used, supplemented with 0.02g of cationic brilliant red 5GN dye, and the staining procedure was carried out according to the method and conditions described in example 4.
The dried dyed acrylic fiber was measured using a K/S colorimeter of UITRASCAN XE, model number, manufactured by precision instruments, Ltd. to obtain a K/S value of 11.09, which is equivalent to the K/S value of the dyed acrylic fiber obtained by dyeing with a fresh anhydrous dyeing medium based on ionic liquid, indicating that the recycled anhydrous dyeing medium supplemented with dye is applicable to the same pigment dyeing process.
The anhydrous dyeing methods of examples 4 to 16 achieve that water is not required to be added in the dyeing process, washing water can be recycled after simple treatment, compared with the traditional dyeing method, the water consumption is reduced by more than 98%, chemical raw materials such as acid, salt and leveling assistant are not required to be added, the consumption is reduced by 100%, the generation of waste water and waste gas is reduced by 100%, the pollution of the dyeing process to the environment is avoided, and the dyeing effect is equivalent to that of the traditional dyeing method. After the same dye is added, the anhydrous dyeing medium based on ionic liquid can be directly used for the next batch of dyeing.
Example 17
The method for recovering the anhydrous dyeing medium based on the ionic liquid comprises the following steps:
step 1) uniformly mixing 46g of the dyed anhydrous dyeing medium containing the cationic brilliant blue RL dye based on the ionic liquid and 67g of carbon tetrachloride in a volume ratio of about 1:1, wherein the anhydrous dyeing medium based on the ionic liquid is mutually soluble with the carbon tetrachloride, and the cationic brilliant blue RL dye is separated out in a solid form;
step 2) carrying out solid-liquid separation on the material obtained in the step 1) by adopting a filter paper filtering method to obtain liquid containing an anhydrous dyeing medium based on ionic liquid and carbon tetrachloride and about 0.92g of cation brilliant blue RL dye solid;
and 3) evaporating carbon tetrachloride in the liquid containing the anhydrous dyeing medium based on the ionic liquid and the carbon tetrachloride obtained in the step 2) through rotary evaporation to obtain the anhydrous dyeing medium based on the ionic liquid without the cation brilliant blue RL dye, and cooling the evaporated carbon tetrachloride to obtain the carbon tetrachloride liquid.
The carbon tetrachloride liquid obtained in the step 3) can be used for recycling the dyeing medium of the next batch.
Dyeing of cotton fibers with reactive blue KNR dye was carried out using the ionic liquid based anhydrous dyeing medium obtained in step 3) above to remove cationic brilliant blue RL dye according to the method and conditions described in example 6. The dried dyed material was measured using a K/S colorimeter of UITRASCAN XE, model number, manufactured by precision instruments, Inc., to obtain a K/S value of 10.26, which is equivalent to the K/S value of dyed acrylic fibers dyed with fresh anhydrous dyeing media based on ionic liquids, and no color deviation was found, indicating that the recycled anhydrous dyeing media are feasible for dyeing other dyes.
Example 18
The method for recovering the anhydrous dyeing medium based on the ionic liquid comprises the following steps:
step 1) uniformly mixing 18g of the ionic liquid-based anhydrous dyeing medium containing the acid scarlet GR dye obtained in the step 5) of the embodiment 10 with 53g of carbon tetrachloride in a volume ratio of about 1:2, wherein the ionic liquid-based anhydrous dyeing medium and the carbon tetrachloride are mutually soluble, and the acid scarlet GR dye is precipitated in a solid form;
step 2) carrying out solid-liquid separation on the material obtained in the step 1) by adopting a filter paper filtering method to obtain liquid containing an anhydrous dyeing medium based on ionic liquid and carbon tetrachloride and about 0.02g of acid scarlet GR dye solid;
and 3) evaporating carbon tetrachloride in the liquid containing the anhydrous dyeing medium based on the ionic liquid and carbon tetrachloride obtained in the step 2) through rotary evaporation to obtain the anhydrous dyeing medium based on the ionic liquid without acid scarlet GR dye, and cooling the evaporated carbon tetrachloride to obtain the carbon tetrachloride liquid.
Example 19
The method for recovering the anhydrous dyeing medium based on the ionic liquid comprises the following steps:
step 1) uniformly mixing 40g of the ionic liquid-based anhydrous dyeing medium containing the active black KN-B dye obtained in the step 5) of the example 13 and 30g of carbon tetrachloride in a volume ratio of about 2:1, wherein the ionic liquid-based anhydrous dyeing medium and the carbon tetrachloride are mutually soluble, and the active black KN-B dye is precipitated in a solid form;
step 2) carrying out solid-liquid separation on the material obtained in the step 1) by adopting a filter paper filtering method to obtain liquid containing an anhydrous dyeing medium based on ionic liquid and carbon tetrachloride and about 0.04g of active black KN-B dye solid;
and 3) evaporating carbon tetrachloride in the liquid containing the ionic liquid-based anhydrous dyeing medium and carbon tetrachloride obtained in the step 2) through rotary evaporation to obtain the ionic liquid-based anhydrous dyeing medium without the active black KN-B dye, and cooling the evaporated carbon tetrachloride to obtain the carbon tetrachloride liquid.
The recycling method of the anhydrous dyeing medium described in embodiments 17 to 19 realizes recycling of the anhydrous dyeing medium, is simple and convenient, and simultaneously realizes recycling of residual dye and carbon tetrachloride, thereby greatly reducing the use cost of the dyeing medium.
Claims (6)
1. An anhydrous dyeing medium based on ionic liquid, characterized in that it contains 1-alkyl-3-methylimidazolium hydrogen sulfate [ C ]nmim]HSO4And 1-alkyl-3-methylimidazolium tetrafluoroborate [ C ]nmim]BF4Water is not contained;
the alkyl group comprises ethyl, butyl or octyl;
the pH value of the anhydrous dyeing medium based on the ionic liquid is 4-5, and 1-alkyl-3-methylimidazole bisulfate [ C ] is adjustednmim]HSO4And 1-alkyl-3-methylimidazolium tetrafluoroborate [ C ]nmim]BF4The composition ratio of (A) to (B).
2. An anhydrous dyeing process using the anhydrous ionic liquid-based dyeing medium according to claim 1, characterized in that it comprises the following steps:
1) preparation of a dyeing medium: using 1-alkyl-3-methylimidazolium hydrogen sulfate [ C ]nmim]HSO4And 1-alkyl-3-methylimidazolium tetrafluoroborate [ C ]nmim]BF4Preparing an anhydrous dyeing medium based on ionic liquid, and controlling the pH value of the dyeing medium to be 4-5;
2) soaking: raising the temperature of the anhydrous dyeing medium based on the ionic liquid obtained in the step 1) to 60-95 ℃, putting the material to be dyed into the anhydrous dyeing medium, and soaking for 1-20 min;
3) dyeing: putting a dye into the material-containing dyeing medium obtained in the step 2), uniformly stirring, keeping the temperature at 60-95 ℃ for 5-20 min, then raising the temperature to be higher than 100 ℃, keeping the temperature for 10-60 min, and dyeing the material, wherein the dye can be dissolved in the ionic liquid-based anhydrous dyeing medium;
4) cooling: reducing the temperature of the dyeing medium of step 3) to below 60 ℃;
5) and (3) post-treatment: taking out the dyed material obtained in the step 4), extruding the dyeing medium carried in the material in an extrusion mode, washing the material and drying.
3. The waterless dyeing method of claim 2, wherein the material to be dyed in step 2) comprises acrylic fiber, wool and cotton.
4. The waterless dyeing method of claim 2, wherein the temperature in step 3) is increased at a constant speed, and the temperature increase rate is 0.5 ℃/min-3 ℃/min.
5. The waterless dyeing method of claim 2, wherein the temperature in step 4) is reduced at a constant speed, and the temperature reduction rate is 0.5 ℃/min-5 ℃/min.
6. The waterless dyeing method of claim 2, wherein the dyeing medium obtained after the dyeing in step 5) can be recycled, and the same dye is added to the used dyeing medium for the next dyeing batch.
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| CN102776790A (en) * | 2012-07-10 | 2012-11-14 | 东华大学 | Waterless dyeing method of dispersed dye |
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