阅读说明：本技术 一种高温环保的化纤染色工艺 (High-temperature environment-friendly chemical fiber dyeing process ) 是由 靳黎伟 沈小伟 王欢 于 2021-08-04 设计创作，主要内容包括：本发明公开了一种高温环保的化纤染色工艺,属于染料技术领域。且该染色工艺包括以下步骤：一、将待染化纤水洗,再浸入色浆中,经过一浸一轧后,得浸轧后的化纤；二、将浸轧后的化纤水洗,皂洗,水洗后,烘干,染色完成。且本发明在染色工艺过程中改变二浸二轧的方式为一浸一轧,减少水的用量,提高环保；在一浸一轧染色过程中引入固色剂,该固定剂具有双键封端,易交联形成一层薄膜,含有苯基,刚性大,提高了形成的薄膜的硬度,提高了染色化纤耐洗牢度和耐晒牢度,且提高了染料的利用率,减少因染料过量使用造成水的污染,且薄膜减少皂洗和水洗过程中染料的脱离,从而降低了皂洗或水洗过程中的水污染。(The invention discloses a high-temperature environment-friendly chemical fiber dyeing process, and belongs to the technical field of dyes. And the dyeing process comprises the following steps: firstly, washing chemical fibers to be dyed, then soaking the chemical fibers into color paste, and obtaining the chemical fibers after padding after one-time soaking and one-time rolling; and secondly, washing the padded chemical fiber with water, soaping, drying and dyeing. In the dyeing process, the mode of two-dipping and two-rolling is changed into one-dipping and one-rolling, so that the consumption of water is reduced, and the environment friendliness is improved; the fixing agent is introduced in the one-dip one-pad dyeing process, has double-bond end capping, is easy to crosslink to form a layer of film, contains phenyl, has high rigidity, improves the hardness of the formed film, improves the washing fastness and the light fastness of the dyed chemical fiber, improves the utilization rate of the dye, reduces the water pollution caused by excessive use of the dye, and reduces the separation of the dye in the soaping and water washing processes, thereby reducing the water pollution in the soaping or water washing processes.)

1. A high-temperature environment-friendly chemical fiber dyeing process is characterized by comprising the following steps: the method comprises the following steps:

firstly, washing chemical fibers to be dyed, immersing the chemical fibers into color paste, adding a color fixing agent when the temperature is raised to 120 ℃, preserving the heat for 20-25min, and then rolling to obtain the chemical fibers after padding;

secondly, washing the padded chemical fiber with water, soaping, washing with water again, and drying to finish dyeing;

the color fixing agent is prepared by the following steps:

mixing tricarboxylic acid, amino-terminated polydimethylsiloxane and glacial acetic acid, adding p-toluenesulfonic acid, stirring and reacting at 78 ℃ for 8 hours, decompressing, steaming, washing and drying in vacuum to obtain an intermediate 1; and (3) uniformly mixing the intermediate 1, methacrylic acid and glacial acetic acid, adding p-toluenesulfonic acid, stirring and reacting at 92 ℃ for 12 hours, decompressing and rotary-steaming, and drying in vacuum to obtain the color fixing agent.

2. The high-temperature environment-friendly chemical fiber dyeing process according to claim 1, characterized in that: in the first step, the temperature of the color paste is 45 ℃ when the color paste is immersed, the bath ratio is 1: 8, the heating rate is 2-3 ℃/min.

3. The high-temperature environment-friendly chemical fiber dyeing process according to claim 1, characterized in that: the soaping conditions in the step two are as follows: the bath ratio is 1: 8, keeping the pH of the soap lotion at 6-7 at 75 ℃ for 12-20 min.

4. The high-temperature environment-friendly chemical fiber dyeing process according to claim 1, characterized in that: in the second step, the drying temperature is controlled at 190-220 ℃, and the drying time is 2-5 min.

5. The high-temperature environment-friendly chemical fiber dyeing process according to claim 1, characterized in that: the color paste comprises the following components in percentage by weight: 18-35% of water-based acrylate, 0.3-0.8% of penetrant, 0.4-0.9% of sodium chloride, 1.5-4.5% of sodium gluconate, 1.5-9.5% of acid dye and the balance of water.

6. The high-temperature environment-friendly chemical fiber dyeing process according to claim 5, characterized in that: the penetrant is fatty alcohol-polyoxyethylene ether penetrant JFC, alkylphenol polyoxyethylene ether penetrant JFC-1 and polyoxyethylene ether compound penetrant JFC-S according to the mass ratio of 1-1.5: 1.2-1.6: 1.5-1.8.

7. The high-temperature environment-friendly chemical fiber dyeing process according to claim 1, characterized in that: the tricarboxylic acid is prepared by the following steps:

mixing the trihydric alcohol, adipic acid and N, N-dimethylformamide uniformly, adding p-toluenesulfonic acid at 82 ℃, reacting for 8 hours, and carrying out reduced pressure rotary evaporation to obtain the tricarboxylic acid.

8. The high-temperature environment-friendly chemical fiber dyeing process according to claim 7, characterized in that: the triol is prepared by the following steps:

mixing p-hydroxymethyl benzaldehyde, benzyl alcohol and glacial acetic acid, cooling to 0 ℃, dropwise adding a mixed solution of concentrated sulfuric acid and glacial acetic acid while stirring, continuously stirring and reacting at 0 ℃ for 36 hours after dropwise adding is completed, then pouring ice water, stirring, filtering, washing with water, and drying in vacuum to obtain the trihydric alcohol.

Technical Field

The invention belongs to the technical field of dyes, and particularly relates to a high-temperature environment-friendly chemical fiber dyeing process.

Background

The dyeing process is a process of dyeing the clothes by the steps of padding, soaping, washing, drying and the like. In the process, a soaping or water washing step consumes a large amount of water, and the water after washing contains dye components, while the traditional dye generally contains chemical components harmful to the environment, so that water pollution and environmental damage are caused. The environment-friendly dye is produced at the same time, meets the following conditions, does not contain or generate harmful aromatic amine, is not carcinogenic, allergic or acute toxic, is limited below the limit after being used, does not contain environmental hormone, does not contain persistent organic pollutants, and does not generate chemical substances polluting the environment. However, the performance of the existing environment-friendly dye in some aspects is far inferior to that of the traditional dye, such as washing fastness, sun fastness and the like, and the market competitiveness of the existing environment-friendly dye is reduced.

Therefore, the invention provides a high-temperature environment-friendly chemical fiber dyeing process, which is used for dyeing by an improved dyeing process, and simultaneously ensures the washing fastness and the light fastness of the dyed chemical fiber on the premise of ensuring that the environment is not polluted.

Disclosure of Invention

The invention aims to provide a high-temperature environment-friendly chemical fiber dyeing process.

The technical problems to be solved by the invention are as follows: solves the pollution problem in the soaping or water washing process in the dyeing process, and improves the washing fastness and the light fastness of the dyed chemical fiber.

The purpose of the invention can be realized by the following technical scheme:

a high-temperature environment-friendly chemical fiber dyeing process comprises the following steps:

firstly, washing chemical fibers to be dyed with water to remove impurities, then soaking the chemical fibers in color paste, and obtaining the chemical fibers after padding after one-time soaking and one-time rolling;

and secondly, washing the padded chemical fiber with water, soaping, drying and dyeing.

Further, the padding condition in the first step is as follows: the immersion temperature was 45 ℃, the bath ratio was 1: and 8, heating at the speed of 2-3 ℃/min, adding a color fixing agent when the temperature is raised to 120 ℃, and keeping the temperature for 20-25 min.

Further, the soaping conditions in the step two are as follows: the bath ratio is 1: 8, keeping the pH of the soap lotion at 6-7 at 75 ℃ for 12-20 min.

Further, the drying temperature in the water washing in the step two is controlled at 190-220 ℃, and the drying time is 2-5 min.

Further, the color paste comprises the following components in percentage by weight: 18-35% of water-based acrylate, 0.3-0.8% of penetrant, 0.4-0.9% of sodium chloride, 1.5-4.5% of sodium gluconate, 1.5-9.5% of acid dye and the balance of water.

Further, the penetrant is fatty alcohol-polyoxyethylene ether penetrant JFC, alkylphenol polyoxyethylene ether penetrant JFC-1 and polyoxyethylene ether compound penetrant JFC-S according to the mass ratio of 1-1.5: 1.2-1.6: 1.5-1.8, and the penetrating agent is used for improving the penetrating, emulsifying, diffusing and antistatic capabilities of the dye.

Further, the fixing agent is prepared by the following steps:

s1, sequentially adding p-hydroxymethylbenzaldehyde, benzyl alcohol and glacial acetic acid into a three-neck flask, uniformly stirring, cooling to 0 ℃, slowly dropwise adding a mixed solution of concentrated sulfuric acid and glacial acetic acid while stirring at the dropping speed of 1 drop/second, continuously stirring at 0 ℃ for reaction for 36 hours after dropwise adding is completed, then pouring ice water, stirring for 50 minutes, filtering, repeatedly washing and filtering a filter cake with the ice water until the filtrate is neutral, and then drying the filter cake in vacuum to constant weight to obtain a ternary alcohol, wherein the dosage ratio of the mixed solution of the p-hydroxymethylbenzaldehyde, the benzyl alcohol, the glacial acetic acid, the concentrated sulfuric acid and the glacial acetic acid is 0.01 mol: 0.021-0.024 mol: 25-35 mL: 7-13mL of mixed solution of concentrated sulfuric acid and glacial acetic acid, wherein the mixed solution of the concentrated sulfuric acid and the glacial acetic acid is prepared from 98% of concentrated sulfuric acid and glacial acetic acid according to a volume ratio of 1-1.4: 3, mixing;

the reaction formula is shown as follows:

s2, adding the triol, the adipic acid and the N, N-dimethylformamide into a three-neck flask, uniformly mixing, controlling the reaction temperature to 82 ℃, adding the p-toluenesulfonic acid, reacting for 8 hours, removing the solvent by reduced pressure rotary evaporation to obtain the tricarboxylic acid, and reacting the alcoholic hydroxyl group with the carboxyl group, wherein the use ratio of the triol, the adipic acid, the N, N-dimethylformamide and the p-toluenesulfonic acid is 0.01 mol: 0.03-0.033 mol: 50-150 mL: 1-3 mg; under the protection of nitrogen gas flow, adding D into a four-neck flask₄And a catalyst benzyl trimethyl amine hydroxide methanol solution (0.5 wt%), heating to 43 ℃ under magnetic stirring, adding a blocking agent, removing residual water and methanol in the system under reduced pressure, continuing to perform an equilibrium reaction for 10 hours when the viscosity of the system is not changed, continuing to raise the temperature to 172 ℃ to destroy the activity of a catalytic center, then cooling to 150 ℃, removing the residual D4 and low-boiling-point substance micromolecules in the reaction under negative pressure to obtain amino-terminated polydimethylsiloxane, and performing ring-opening polymerization reaction by utilizing the anion of D4, wherein the blocking agent is 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane, and the dosage ratio of the D4, the catalyst and the blocking agent is 50 g: 0.5 g: 4-8 g;

the reaction formula is as follows:

s3, uniformly mixing tricarboxylic acid, amino-terminated polydimethylsiloxane and glacial acetic acid, adding p-toluenesulfonic acid, stirring and reacting for 8 hours at 78 ℃, cooling to 35 ℃, decompressing and steaming, repeatedly washing for 3 times by deionized water, and drying in vacuum at 40 ℃ to constant weight to obtain an intermediate 1, wherein the carboxyl and amino reactions are utilized, and the dosage ratio of the tricarboxylic acid, the amino-terminated polydimethylsiloxane, the glacial acetic acid and the p-toluenesulfonic acid is 0.01 mol: 0.032-0.034 mol: 50-150 mL: 0.5-1 g; uniformly mixing the intermediate 1, methacrylic acid and glacial acetic acid, adding p-toluenesulfonic acid, stirring and reacting at 92 ℃ for 12h, cooling to 30 ℃, decompressing and rotary steaming, drying at 40 ℃ in vacuum to constant weight to obtain a color fixing agent, and reacting by using amino and carboxyl, wherein the dosage ratio of the intermediate 1, the methacrylic acid, the glacial acetic acid and the p-toluenesulfonic acid is 0.01 mol: 0.031-0.033 mol: 50-150 mL: 0.5-1 g.

The reaction is shown below:

the invention has the beneficial effects that:

firstly, the dyeing process changes the mode of two-dipping and two-rolling into one-dipping and one-rolling, reduces the consumption of water and improves the environmental protection; secondly, the bath ratio used in the soaping and water washing processes is low, and the using amount of water is reduced; finally, the introduction of the color fixing agent is utilized in the one-dip one-pad dyeing process, so that on one hand, the dyeing process efficiency is improved, the utilization rate of the dye is improved, the excessive dye is reduced, the pollution caused by water is reduced, the washing fastness and the light fastness of the dyed chemical fiber are improved, on the other hand, the separation of the acid dye in the soaping and washing processes is reduced, and the water pollution in the soaping or washing processes is reduced.

The fixing agent is obtained by gradually reacting tricarboxylic acid, amino-terminated polydimethylsiloxane and methacrylic acid, the fixing agent has double-bond terminated end, a layer of film is easily formed on the surface of the chemical fiber through crosslinking, and the tricarboxylic acid contains triphenyl, has high rigidity, improves the hardness of the film, and enables the film to be wear-resistant, so that the dyeing chemical fiber is prevented from fading, and the washing fastness and the light fastness of the dyeing chemical fiber are improved.

In conclusion, the dyeing process provided by the invention has the advantages of less water consumption, high dye utilization rate, reduction of environmental pollution in the soaping or water washing process, and good washing fastness and light fastness of the obtained dyed chemical fiber.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1:

the color fixing agent is prepared by the following steps:

s1, sequentially adding 0.01mol of p-hydroxy methyl benzaldehyde, 0.021mol of benzyl alcohol and 25mL of glacial acetic acid into a three-neck flask, uniformly stirring, cooling to 0 ℃, slowly dropwise adding 7mL of a mixed solution of concentrated sulfuric acid and glacial acetic acid while stirring at a speed of 1 drop/second, continuously stirring at 0 ℃ for reacting for 36 hours after dropwise adding is completed, then pouring ice water, stirring for 50 minutes, filtering, repeatedly washing and filtering a filter cake with the ice water until the filtrate is neutral, and then drying the filter cake in vacuum to constant weight to obtain the trihydric alcohol, wherein the mixed solution of the concentrated sulfuric acid and the glacial acetic acid is prepared by mixing 98% of concentrated sulfuric acid and glacial acetic acid according to a volume ratio of 1: 3, mixing;

s2, adding 0.01mol of trihydric alcohol, 0.03mol of adipic acid and 50mLN, N-dimethylformamide into a three-neck flask, uniformly mixing, controlling the reaction temperature to 82 ℃, adding 1mg of p-toluenesulfonic acid, reacting for 8 hours, removing the solvent by rotary evaporation under reduced pressure to obtain tribasic carboxylic acid, and reacting with alcoholic hydroxyl and carboxyl; under the protection of nitrogen gas flow, 50gD of the mixture was added into a four-neck flask₄And 0.5g of catalyst benzyltrimethyl ammonium hydroxide methanol solution (0.5 wt%), heating to 43 ℃ under magnetic stirring, adding 4g of end capping agent, removing residual water and methanol in the system under reduced pressure, continuing the equilibrium reaction for 10 hours when the viscosity of the system is not changed, continuing to raise the temperature to 172 ℃ to destroy the activity of a catalytic center, then cooling to 150 ℃, and removing residual D in the reaction under negative pressure₄Monomer and low-boiling-point substance micromolecule to obtain amino-terminated polydimethylsiloxane, wherein the end-capping agent is 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane;

s3, uniformly mixing 0.01mol of tricarboxylic acid, 0.032mol of amino-terminated polydimethylsiloxane and 50mL of glacial acetic acid, adding 0.5g of p-toluenesulfonic acid, stirring and reacting at 78 ℃ for 8h, cooling to 35 ℃, decompressing and rotary steaming, repeatedly washing for 3 times with deionized water, and drying in vacuum at 40 ℃ to constant weight to obtain an intermediate 1; 0.01mol of intermediate 1, 0.031mol of methacrylic acid and 50mL of glacial acetic acid are mixed uniformly, 0.5g of p-toluenesulfonic acid is added, the mixture is stirred and reacts for 12 hours at the temperature of 92 ℃, the mixture is cooled to 30 ℃ and is decompressed and steamed in a rotary manner, and the mixture is dried in vacuum at the temperature of 40 ℃ to constant weight, so that the color fixing agent is obtained.

Example 2:

the color fixing agent is prepared by the following steps:

s1, sequentially adding 0.01mol of p-hydroxymethylbenzaldehyde, 0.024mol of benzyl alcohol and 35mL of glacial acetic acid into a three-neck flask, uniformly stirring, cooling to 0 ℃, slowly dropwise adding 13mL of a mixed solution of concentrated sulfuric acid and glacial acetic acid while stirring at a speed of 1 drop/second, continuously stirring at 0 ℃ for reacting for 36 hours after dropwise adding is completed, then pouring ice water, stirring for 50 minutes, filtering, repeatedly washing and filtering a filter cake with the ice water until the filtrate is neutral, and then drying the filter cake in vacuum to constant weight to obtain the trihydric alcohol, wherein the mixed solution of the concentrated sulfuric acid and the glacial acetic acid is prepared from 98% of concentrated sulfuric acid and glacial acetic acid according to a volume ratio of 1.4: 3, mixing;

s2, adding 0.01mol of triol, 0.033mol of adipic acid and 150mLN, N-dimethylformamide into a three-neck flask, uniformly mixing, controlling the reaction temperature to 82 ℃, adding 3mg of p-toluenesulfonic acid, reacting for 8 hours, and removing the solvent by rotary evaporation under reduced pressure to obtain tricarboxylic acid; under the protection of nitrogen gas flow, 50gD of the mixture was added into a four-neck flask₄And 0.5g of catalyst benzyltrimethyl ammonium hydroxide methanol solution (0.5 wt%), heating to 43 ℃ under magnetic stirring, adding 8g of end capping agent, removing residual water and methanol in the system under reduced pressure, continuing the equilibrium reaction for 10 hours when the viscosity of the system is not changed, continuing to raise the temperature to 172 ℃ to destroy the activity of a catalytic center, then cooling to 150 ℃, and removing residual D in the reaction under negative pressure₄Monomer and low-boiling-point substance micromolecule to obtain amino-terminated polydimethylsiloxane, wherein the end-capping agent is 1, 3-bis (3-aminopropyl) -1,1,3, 3-tetramethyldisiloxane;

s3, uniformly mixing 0.01mol of tricarboxylic acid, 0.034mol of amino-terminated polydimethylsiloxane and 150mL of glacial acetic acid, adding 1g of p-toluenesulfonic acid, stirring and reacting at 78 ℃ for 8h, cooling to 35 ℃, decompressing and rotary steaming, repeatedly washing for 3 times with deionized water, and drying in vacuum at 40 ℃ to constant weight to obtain an intermediate 1; uniformly mixing 0.01mol of the intermediate 1, 0.033mol of methacrylic acid and 150mL of glacial acetic acid, adding 1g of p-toluenesulfonic acid, stirring and reacting at 92 ℃ for 12h, cooling to 30 ℃, decompressing and rotary steaming, and drying in vacuum at 40 ℃ to constant weight to obtain the color fixing agent.

Example 3:

the color paste comprises the following components in percentage by weight: 18% of water-based acrylate, 0.3% of penetrant, 0.4% of sodium chloride, 1.5% of sodium gluconate, 1.5% of acid dye and the balance of water, wherein the penetrant is fatty alcohol-polyoxyethylene ether penetrant JFC, alkylphenol-polyoxyethylene ether penetrant JFC-1 or polyoxyethylene ether compound penetrant JFC-S according to the mass ratio of 1: 1.2: 1.5.

The preparation method comprises the following steps: stirring the components at 750r/min for 35 min.

Example 4:

the color paste comprises the following components in percentage by weight: 26% of water-based acrylate, 0.6% of penetrant, 0.6% of sodium chloride, 2% of sodium gluconate, 6% of acid dye and water in balance, wherein the penetrant is fatty alcohol-polyoxyethylene ether penetrant JFC, alkylphenol polyoxyethylene ether penetrant JFC-1 and polyoxyethylene ether compound penetrant JFC-S according to a mass ratio of 1.2: 1.3: 1.6.

The preparation method comprises the following steps: stirring the components at 750r/min for 35 min.

Example 5:

the color paste comprises the following components in percentage by weight: 35% of water-based acrylate, 0.8% of penetrant, 0.9% of sodium chloride, 4.5% of sodium gluconate, 9.5% of acid dye and the balance of water, wherein the penetrant is fatty alcohol-polyoxyethylene ether penetrant JFC, alkylphenol-polyoxyethylene ether penetrant JFC-1 or polyoxyethylene ether compound penetrant JFC-S according to the mass ratio of 1.5: 1.6: 1.8.

The preparation method comprises the following steps: stirring the components at 750r/min for 35 min.

Example 6:

a high-temperature environment-friendly chemical fiber dyeing process comprises the following steps:

firstly, washing chemical fibers to be dyed with water to remove impurities, then soaking the chemical fibers into color paste, and obtaining the chemical fibers after padding after one-time soaking and one-time rolling, wherein the padding conditions are as follows: the immersion temperature was 45 ℃, the bath ratio was 1: 8, heating up to 120 ℃ at the heating-up speed of 3 ℃/min, adding the color fixing agent prepared in the example 1, and keeping the temperature for 20 min;

washing the padded chemical fiber with water, soaping, drying and dyeing, wherein the soaping conditions are as follows: the bath ratio is 1: 8, keeping the pH value of the soap lotion at 6 for 12min at 75 ℃; the drying temperature is controlled at 190 ℃ and the drying time is 2 min.

Example 7:

a high-temperature environment-friendly chemical fiber dyeing process comprises the following steps:

firstly, washing chemical fibers to be dyed with water to remove impurities, then soaking the chemical fibers into color paste, and obtaining the chemical fibers after padding after one-time soaking and one-time rolling, wherein the padding conditions are as follows: the immersion temperature was 45 ℃, the bath ratio was 1: 8, heating up at the speed of 2 ℃/min, adding the color fixing agent prepared in the example 2 when the temperature is raised to 120 ℃, and keeping the temperature for 25 min;

washing the padded chemical fiber with water, soaping, drying and dyeing, wherein the soaping conditions are as follows: the bath ratio is 1: 8, keeping the pH value of the soap lotion at 6.5 and keeping the temperature at 75 ℃ for 16 min; the drying temperature is controlled at 200 ℃ and the drying time is 5 min.

Example 8:

a high-temperature environment-friendly chemical fiber dyeing process comprises the following steps:

firstly, washing chemical fibers to be dyed with water to remove impurities, then soaking the chemical fibers into color paste, and obtaining the chemical fibers after padding after one-time soaking and one-time rolling, wherein the padding conditions are as follows: the immersion temperature was 45 ℃, the bath ratio was 1: 8, heating up to 120 ℃ at the heating-up speed of 3 ℃/min, adding the color fixing agent prepared in the example 1, and keeping the temperature for 25 min;

washing the padded chemical fiber with water, soaping, drying and dyeing, wherein the soaping conditions are as follows: the bath ratio is 1: 8, keeping the pH value of the soap lotion at 7 for 20min at 75 ℃; the drying temperature is controlled at 220 ℃ and the drying time is 5 min.

Comparative example 1:

the color fixing agent is prepared by the following steps:

s1, sequentially adding 0.01mol of p-hydroxymethylbenzaldehyde, 0.021 benzyl alcohol and 25mL of glacial acetic acid into a three-neck flask, uniformly stirring, cooling to 0 ℃, slowly dropwise adding 7mL of a mixed solution of concentrated sulfuric acid and glacial acetic acid while stirring at a speed of 1 drop/second, continuously stirring at 0 ℃ for reacting for 36 hours after dropwise adding is completed, then pouring ice water, stirring for 50 minutes, filtering, repeatedly washing and filtering a filter cake with the ice water until the filtrate is neutral, and then drying the filter cake in vacuum to constant weight to obtain the trihydric alcohol, wherein the mixed solution of the concentrated sulfuric acid and the glacial acetic acid is prepared by mixing 98% of concentrated sulfuric acid and glacial acetic acid according to a volume ratio of 1: 3, mixing;

s2, adding 0.01mol of trihydric alcohol, 0.03mol of adipic acid and 50mLN, N-dimethylformamide into a three-neck flask, uniformly mixing, controlling the reaction temperature to 82 ℃, adding 1-3mg of p-toluenesulfonic acid, reacting for 8 hours, and removing the solvent by rotary evaporation under reduced pressure to obtain tribasic carboxylic acid;

s3, uniformly mixing 0.01mol of tricarboxylic acid, 0.031mol of methacrylic acid and 50mL of glacial acetic acid, adding 0.5g of p-toluenesulfonic acid, stirring and reacting at 92 ℃ for 12h, cooling to 30 ℃, decompressing and rotary steaming, and drying in vacuum at 40 ℃ to constant weight to obtain the color fixing agent.

Comparative example 2:

a dyeing process comprising the steps of:

firstly, washing chemical fibers to be dyed with water to remove impurities, then soaking the chemical fibers into color paste, and obtaining the chemical fibers after padding after one-time soaking and one-time rolling, wherein the padding conditions are as follows: the immersion temperature was 45 ℃, the bath ratio was 1: 8, heating up to 120 ℃ at the speed of 2 ℃/min, adding the intermediate 1 prepared in the example 1, and keeping the temperature for 20 min;

washing the padded chemical fiber with water, soaping, drying and dyeing, wherein the soaping conditions are as follows: the bath ratio is 1: 8, keeping the pH value of the soap lotion at 6 for 12min at 75 ℃; the drying temperature is controlled at 190 ℃ and the drying time is 2 min.

Comparative example 3:

a dyeing process comprising the steps of:

firstly, washing chemical fibers to be dyed with water to remove impurities, then soaking the chemical fibers into color paste, and obtaining the chemical fibers after padding after one-time soaking and one-time rolling, wherein the padding conditions are as follows: the immersion temperature was 45 ℃, the bath ratio was 1: 8, heating up to 120 ℃ at the heating rate of 2 ℃/min, adding the intermediate 1 prepared in the comparative example 1, and keeping the temperature for 25 min;

washing the padded chemical fiber with water, soaping, drying and dyeing, wherein the soaping conditions are as follows: the bath ratio is 1: 8, keeping the pH value of the soap lotion at 7 for 20min at 75 ℃; the drying temperature is controlled at 220 ℃ and the drying time is 5 min.

Example 9:

the dyed chemical fibers obtained in examples 6 to 8 and comparative examples 1 to 3 were woven into textiles, cut into 10cm × 10cm samples, and subjected to the following performance tests:

the color fastness to washing test refers to the color fastness to washing test and refers to GB/T3921-2008 'color fastness to washing test for textiles';

the light color fastness test refers to GB/T8426-1998 color fastness to light test of textiles;

the color fastness to rubbing is tested according to GB/T3920-2008 'color fastness to rubbing' test of textiles;

the data obtained from the test are shown below.

As can be seen from the data on the wash fastness, the rubbing fastness and the light fastness of examples 6 to 8 and comparative examples 1 to 8, the corresponding properties of the chemical fibers after the dyes obtained in examples 6 to 8 are better than those of the chemical fibers after the dyes obtained in comparative examples 1 to 3 in terms of the wash fastness, the rubbing fastness and the light fastness.

In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.