A method for preparing a fatty amine polyoxyethylene ether sulfonate leveling agent and its application in dyeing and fixing nylon fabrics in a single bath.

Abstract

This invention discloses a method for preparing a fatty amine polyoxyethylene ether sulfonate leveling agent and its application in the dyeing and fixing of nylon fabrics in a co-bath process. The preparation method includes vacuum dehydrating a fatty amine polyoxyethylene ether, then sequentially adding urea and aminosulfonic acid and mixing thoroughly. The mixture is then heated until the hydroxyl conversion rate of the reaction system is ≥92%, yielding a fatty amine polyoxyethylene ether sulfonate. After cooling the reaction system, an organic solvent and deionized water are added for dilution, and the pH is adjusted to 6.5-7.5 to obtain the fatty amine polyoxyethylene ether sulfonate leveling agent. The hydroxyl value of the fatty amine polyoxyethylene ether is 52 mg KOH / g-56 mg KOH / g, and the molar ratio of the terminal hydroxyl groups of aminosulfonic acid to the fatty amine polyoxyethylene ether is 1.8-2:1. The fatty amine polyoxyethylene ether sulfonate leveling agent prepared by this method avoids the introduction of free strong acid radicals and can be used in a co-bath with an acidic fixing agent, exhibiting excellent leveling performance and fixing effect.

Description

Technical Field

[0001] This invention relates to the field of textile auxiliaries technology, and in particular to a method for preparing a fatty amine polyoxyethylene ether sulfonate leveling agent and its application in dyeing and fixing nylon fabrics in the same bath. Background Technology

[0002] In acid dyeing processes for protein fibers (wool, silk) and polyamide fibers (nylon), the amino groups on the fiber surface readily protonate and become positively charged under acidic dyeing conditions, creating a strong electrostatic attraction with anionic acid dyes. Without control, this rapid dyeing in the initial (low-temperature) stage can easily lead to severe color variations and spots. Traditional acid leveling agents primarily rely on petrochemical raw materials, most notably traditional fatty amine polyoxyethylene ethers (such as AC-1810 and Pingpingjia O). While these agents can delay dyeing through the solubilizing effect of nonionic EO chains, in acidic environments (pH 4.0-5.5), the central tertiary amine nitrogen atom readily protonates and becomes positively charged. This leads to an industry pain point: after dyeing, fixing agents are added to improve wet rubbing fastness and washing fastness. However, if traditional cationic / nonionic leveling agents are mixed with anionic fixing agents in the same bath, and if the compatibility is poor, the two will produce severe precipitation, which will affect the fixing efficiency and there is a risk of fixing spots in the later stage. It is also very easy to produce defects such as hanging on the wall, tar spots (color spots) and hardening of the fabric hand feel.

[0003] Therefore, existing traditional processes have to adopt a multi-step process of "dyeing → draining and washing → fixing": 1) Dyeing stage: add dye, leveling agent, and acid-releasing agent, heat to 95~100℃ and keep warm for 30~60 minutes, then cool down to below 50℃ and drain; 2) Washing stage: wash in clean water at room temperature for 5~10 minutes, then drain, then add another tank of clean water, and add detergent / soap if necessary to clean the floating color; 3) Fixing stage: add acidic fixing agent, heat to 70~80℃ and keep warm for 20~30 minutes, drain, and dehydrate. The traditional process has the following prominent problems: 1) High energy and water consumption: After dyeing, high-temperature drainage and multiple water washing are required, resulting in huge consumption of water, electricity and steam; 2) Low production efficiency: Dyeing-washing-fixing are carried out in steps, with a total time of 3 to 4 hours; 3) Dyeing quality risk: Temperature fluctuations and mechanical friction during the drainage and washing process can easily lead to fabric abrasion and a decrease in color fastness; 4) Large wastewater discharge: Each batch generates 3 to 4 tanks of high-color and high-COD wastewater, which puts great pressure on environmental protection. Summary of the Invention

[0004] To adapt to the dyeing and fixing process of nylon fabrics in a single bath, traditional fatty amine polyoxyethylene ethers typically require modification. During the research and development process, the inventors discovered that carboxyl-modified fatty amine polyoxyethylene ethers have carboxyl groups that are weakly acidic. In an acidic dyeing bath environment with pH < 5.0, these groups undergo extensive protonation, transforming into electrically neutral -COOH. The molecule loses its anionic charge shielding effect, exposing the internal tertiary amine cations and re-exhibiting cationic properties. When mixed with anionic fixing agents, this results in rapid flocculation and precipitation. It is only compatible with anionic fixing agents in a neutral environment and cannot meet the requirements for simultaneous use in acidic dyeing baths. Furthermore, phosphate-modified fatty amine polyoxyethylene ethers exhibit highly susceptible hydrolytic breakage of their phosphate ester bonds in high-temperature acidic dyeing baths. When the cationic groups are removed and become ineffective, the auxiliary agent reverts to a cationic structure, losing its compatibility and stability with anionic fixing agents. Compared to the two mentioned above, aminosulfonic acid sulfonated modified fatty amine polyoxyethylene ethers have better compatibility with acidic fixing agents. However, in the preparation of traditional fatty amine polyoxyethylene ether sulfonates, aminosulfonic acid is usually used as the sulfation agent and urea as the catalyst. Under nitrogen protection, the fatty amine polyoxyethylene ether is first neutralized with an acid (sulfuric acid, hydrochloric acid, or acetic acid) before undergoing a sulfation reaction with aminosulfonic acid. However, this "first acid neutralization" step introduces a large amount of free strong acid anions (SO4) into the system. 2- Cl - CH3COO - These strong acid radicals pose the following risks: 1) Competitive electrostatic repulsion with anionic fixing agents: Anionic fixing agents (such as bisphenol sulfonate fixing agents) rely on the negative charge of the sulfonic acid group / sulfate ester group to combine with the dye anion to achieve color fixation. When a large number of foreign strong acid radicals (SO4) are present in the system... 2- Cl - CH3COO - When these strong acid radicals compete with the fixing agent anions for positive charge sites on the fiber surface, they simultaneously increase the ionic strength of the dye bath, compress the electric double layer, and disrupt the charge shielding balance of the salt structure within the leveling agent molecule, leading to electrostatic flocculation between the leveling agent and the fixing agent. 2) High temperature and high salt conditions exacerbate sedimentation: In acidic dye baths (pH 4.0~5.5), residual SO42-... 2- / Cl - In synergy with electrolytes (sodium sulfate, salt), the ionic strength of the solution far exceeds the critical value, the micelle structure is destroyed, and the leveling agent molecules change from a dispersed state to an aggregated state, flocculating and precipitating with the anionic fixing agent. Based on this, the purpose of this invention is to provide a method for preparing a fatty amine polyoxyethylene ether sulfonate leveling agent without strong acid radical residue and its application in the dyeing and fixing of nylon fabrics in a co-bath. The fatty amine polyoxyethylene ether sulfonate leveling agent prepared by the method of this invention avoids the introduction of free strong acid radicals and can be used in a co-bath with acidic fixing agents, exhibiting excellent leveling performance and fixing effect.

[0005] To achieve the above objectives, the present invention provides a method for preparing a fatty amine polyoxyethylene ether sulfonate leveling agent, comprising: S1. Vacuum dehydration treatment of fatty amine polyoxyethylene ether is carried out, and then urea and aminosulfonic acid are added in sequence and mixed evenly. The reaction is carried out at a temperature until the hydroxyl conversion rate of the reaction system is ≥92% to obtain fatty amine polyoxyethylene ether sulfonate. S2. After cooling the reaction system, add an organic solvent, then add deionized water to dilute to the target solid content, and adjust the pH to 6.5~7.5 to obtain aliphatic amine polyoxyethylene ether sulfonate leveling agent. The hydroxyl value of the fatty amine polyoxyethylene ether is 52mgKOH / g~56mgKOH / g, and the molar ratio of aminosulfonic acid to the terminal hydroxyl group of the fatty amine polyoxyethylene ether is 1.8~2:1.

[0006] Compared with the prior art, the present invention performs vacuum dehydration on the fatty amine polyoxyethylene ether before the sulfation reaction to reduce the influence of moisture in the raw materials on the sulfation reaction; at the same time, it uses an aminosulfonic acid-urea system to directly perform hydroxysulfation, without the need to acidify the amine groups with sulfuric acid, hydrochloric acid or acetic acid in advance, thereby reducing the low molecular weight inorganic / organic counterions and electrolyte load introduced by the pre-neutralization step, which is beneficial to improving the system stability when compounded with anionic acidic fixing agents. This invention uses fatty amine polyoxyethylene ether with a hydroxyl value of 52 mg KOH / g to 56 mg KOH / g, and controls the molar ratio of aminosulfonic acid to the terminal hydroxyl groups of the fatty amine polyoxyethylene ether to be 1.8 to 2:1. An appropriate excess of aminosulfonic acid is used to enhance the driving force and group conversion degree of the target sulfation reaction, and the hydroxyl conversion rate in the reaction system is controlled to be ≥92%, thereby effectively avoiding residual unreacted hydroxyl residues and residual cation defects caused by incomplete modification. Finally, the pH is adjusted to 6.5 to 7.5 to further eliminate any trace amounts of free acid that may be present in the system, thus further eliminating the influence of free acid on the subsequent dyeing and fixing processes. Therefore, the fatty amine polyoxyethylene ether sulfonate leveling agent prepared by the method of this invention has no strong acid radical residues and can be used in the same bath with acidic fixing agents, exhibiting excellent leveling performance and fixing effect.

[0007] Further, the present invention comprises, by weight parts, 100 parts of fatty amine polyoxyethylene ether, 1.5 to 4.5 parts of urea, and 16.5 to 19.5 parts of aminosulfonic acid. Specifically, the weight parts of urea may be, but are not limited to, 1.5 parts, 2.0 parts, 2.5 parts, 3.0 parts, 3.5 parts, 4.0 parts, or 4.5 parts; and the weight parts of aminosulfonic acid may be, but are not limited to, 16.5 parts, 17.0 parts, 17.5 parts, 18.0 parts, 18.5 parts, 19.0 parts, or 19.5 parts.

[0008] Furthermore, the fatty amine polyoxyethylene ether of the present invention has 12 to 18 carbon atoms and 10 to 25 polyoxyethylene additions.

[0009] Furthermore, the vacuum dehydration treatment of the present invention includes treatment at a vacuum degree ≥0.09 MPa and a temperature of 90℃~100℃ for 0.5~3 hours. Specifically, the temperature of the vacuum dehydration treatment can be, but is not limited to, 90℃, 91℃, 92℃, 93℃, 94℃, 95℃, 96℃, 97℃, 98℃, 99℃, or 100℃, and the time can be, but is not limited to, 0.5 hours, 1 hour, 1.5 hours, 2 hours, 2.5 hours, or 3 hours. Under these conditions, trace amounts of free water in the raw materials can be effectively removed, thereby reducing the impact of moisture on the reaction system and improving catalytic efficiency and raw material conversion rate.

[0010] Furthermore, the heating reaction of the present invention includes raising the system temperature to 125°C~135°C and holding it at that temperature for 3.5h~5h. Specifically, the temperature of the heating reaction can be, but is not limited to, 125°C, 126°C, 127°C, 128°C, 129°C, 130°C, 131°C, 132°C, 133°C, 134°C, or 135°C; the holding time can be, but is not limited to, 3.5h, 4h, 4.5h, or 5h.

[0011] Furthermore, the substance used to adjust the pH in this invention is at least one of ammonia and triethanolamine.

[0012] Furthermore, the organic solvent of the present invention is selected from ethylene glycol ethers. Specifically, ethylene glycol ethers include, but are not limited to, at least one of ethylene glycol methyl ether, ethylene glycol ethyl ether, ethylene glycol butyl ether, ethylene glycol propyl ether, ethylene glycol hexyl ether, diethylene glycol methyl ether, diethylene glycol ethyl ether, diethylene glycol butyl ether, triethylene glycol methyl ether, triethylene glycol ethyl ether, and triethylene glycol butyl ether. More specifically, the content of the organic solvent in the fatty amine polyoxyethylene ether sulfonate leveling agent of the present invention is 15% to 20%.

[0013] Furthermore, the solid content of the fatty amine polyoxyethylene ether sulfonate leveling agent of the present invention is 30% to 60%. Specifically, the solid content of the fatty amine polyoxyethylene ether sulfonate leveling agent may be, but is not limited to, 30%, 35%, 40%, 45%, 50%, 55%, or 60%.

[0014] The second aspect of this invention provides the application of the fatty amine polyoxyethylene ether sulfonate leveling agent prepared by the aforementioned method in the dyeing and fixing process of nylon fabrics, comprising: placing the nylon fabric in a dye bath at room temperature, then adding the fatty amine polyoxyethylene ether sulfonate leveling agent, and after it is evenly dispersed, adding an acid dye or a metal complex dye, adjusting the pH of the dye bath to 4.5~6.5, raising the temperature to 75~85℃ at a rate of 1℃ / min~3℃ / min, then slowly adding an acid fixing agent over a period of 25min~35min, and after the acid fixing agent has been added, raising the temperature to 95~105℃ at a rate of 2℃ / min~3℃ / min and holding it at that temperature for 20min~40min, and finally cooling the temperature to 40℃~50℃ to drain the solution and wash with water.

[0015] The fatty amine polyoxyethylene ether sulfonate leveling agent prepared by this invention is particularly suitable for dyeing and fixing nylon fibers and their blended fabrics in a single bath, and is also suitable for weakly acidic dyes and metal complex dyes (neutral dyes). The temperature-controlled and slow-dyeing characteristics of the leveling agent of this invention are highly matched with the dyeing characteristics of weakly acidic dyes, which can significantly improve the leveling properties, and the color difference ΔE can be controlled to a minimum of 0.31. Metal complex dyes are formed by complexing dye molecules with metals such as chromium and cobalt in a certain proportion. They can be dyed in neutral or weakly acidic baths (pH 5.0~6.5), with excellent color fastness and minimal damage to fibers. These dyes have a moderate dyeing rate, good leveling properties, and when combined with the leveling agent of this invention, the system has high stability and excellent single-bath fixing effect.

[0016] Furthermore, the liquor ratio for dyeing and fixing in the same bath according to the present invention is 1:8 to 20. Specifically, the liquor ratio can be, but is not limited to, 1:8, 1:10, 1:12, 1:14, 1:16, 1:18, or 1:20.

[0017] Furthermore, the amount of dye used in this invention is 0.5~5.0% owf, the amount of fatty amine polyoxyethylene ether sulfonate leveling agent is 0.5~3.0% owf, and the amount of acidic fixing agent is 1.0~5.0% owf. Specifically, the amount of dye used may be, but is not limited to, 0.5% owf, 1% owf, 1.5% owf, 2% owf, 2.5% owf, 3% owf, 3.5% owf, 4% owf, 4.5% owf, or 5% owf; the amount of fatty amine polyoxyethylene ether sulfonate leveling agent used may be, but is not limited to, 0.5% owf, 1% owf, 1.5% owf, 2% owf, 2.5% owf, or 3% owf; and the amount of acidic fixing agent used may be, but is not limited to, 1% owf, 1.5% owf, 2% owf, 2.5% owf, 3% owf, 3.5% owf, 4% owf, 4.5% owf, or 5% owf.

[0018] Furthermore, the acidic fixing agent of the present invention is selected from bisphenol-type fixing agents. Bisphenol-type fixing agents contain multiple sulfonic acid groups (-SO3) in their molecular structure. - The bisphenol type fixing agent, like the ammonium sulfate salt at the end of the leveling agent of this invention, belongs to the strongly acidic anionic group. After sulfation, the leveling agent of this invention introduces a strongly acidic anionic sulfate group at the end of the polyoxyethylene chain, which can reduce the net cationic characteristics exhibited by the original aliphatic amine polyoxyethylene ether in acidic media, thereby reducing the tendency to form insoluble ionic complexes with anionic acidic fixing agents and improving compatibility stability. It can coexist stably under extreme conditions of pH 4.5, salt content of 15 g / L, and 98°C, without precipitation, stratification, or wall adhesion, exhibiting excellent co-bath performance. Furthermore, the bisphenol type fixing agent has a large molecular weight, containing multiple benzene ring conjugated structures and sulfonic acid groups, which can combine with sulfonic acid groups, amino groups, and other groups in acidic dye molecules through multiple interactions such as hydrogen bonds, van der Waals forces, and ionic bonds, forming a dense network protective film on the fiber surface. After co-bath fixing with the bisphenol type fixing agent, the washing fastness of nylon fabrics can reach grade 4-5, which is superior to other types of fixing agents. Detailed Implementation

[0019] To better illustrate the purpose, technical solution, and beneficial effects of this invention, the invention will be further described below with reference to specific embodiments. It should be noted that the methods described below are further explanations of this invention and should not be construed as limiting it.

[0020] Example 1 This embodiment provides a method for preparing a fatty amine polyoxyethylene ether sulfonate leveling agent, comprising the following steps: S1. Add octadecylamine polyoxyethylene ether (EO addition number 25, hydroxyl value 53mgKOH / g) to a pressure-resistant reactor equipped with stirring, temperature control, vacuum, and nitrogen protection. Heat to 90℃ and dehydrate for 1.5h under vacuum ≥0.09MPa. Seal and set aside for later use. Take 100g of vacuum-dehydrated octadecylamine polyoxyethylene ether (EO addition number 25, hydroxyl value 53mgKOH / g), add 2.5g of urea, start stirring, and then add 17.4g of aminosulfonic acid and mix evenly (molar ratio of aminosulfonic acid to octadecylamine polyoxyethylene ether terminal hydroxyl group is 1.9:1). Heat to 130℃ and react for 4.5h. The hydroxyl conversion rate of the reaction system is ≥92%, and octadecylamine polyoxyethylene ether sulfonate is obtained. S2. After cooling the reaction system to 70°C, add ethylene glycol methyl ether (15% of the leveling agent), then add deionized water to dilute to the target solid content. Adjust the pH to 7.0 with triethanolamine to obtain a yellow, transparent, viscous liquid with a solid content of about 40%, which is octadecylamine polyoxyethylene ether sulfonate leveling agent.

[0021] Example 2 This embodiment provides a method for preparing a fatty amine polyoxyethylene ether sulfonate leveling agent, comprising the following steps: S1. Add octadecylamine polyoxyethylene ether (EO addition number 25, hydroxyl value 53 mgKOH / g) to a pressure-resistant reactor equipped with stirring, temperature control, vacuum, and nitrogen protection. Heat to 90℃ and dehydrate for 1.5h under vacuum ≥0.09MPa. Seal and set aside for later use. Take 100g of octadecylamine polyoxyethylene ether (EO addition number 25, hydroxyl value 53 mgKOH / g) that has been vacuum dehydrated, then add 4.0g of urea, start stirring, and then add 18.3g of aminosulfonic acid and mix evenly (molar ratio of aminosulfonic acid to octadecylamine polyoxyethylene ether terminal hydroxyl group is 2:1). Heat to 133℃ and react for 4h. The hydroxyl conversion rate of the reaction system is ≥92%, and octadecylamine polyoxyethylene ether sulfonate is obtained. S2. After cooling the reaction system to 70°C, add ethylene glycol methyl ether (15% of the leveling agent), then add deionized water for dilution, and adjust the pH to 7.0 with triethanolamine to obtain a yellow, transparent, viscous liquid with a solid content of about 40%, which is octadecylamine polyoxyethylene ether sulfonate leveling agent.

[0022] Example 3 This embodiment provides a method for preparing a fatty amine polyoxyethylene ether sulfonate leveling agent, comprising the following steps: S1. Add octadecylamine polyoxyethylene ether (EO addition number 25, hydroxyl value 53 mgKOH / g) to a pressure-resistant reactor equipped with stirring, temperature control, vacuum, and nitrogen protection. Heat to 90℃ and dehydrate for 1.5h under vacuum ≥0.09MPa. Seal and set aside for later use. Take 100g of vacuum-dehydrated octadecylamine polyoxyethylene ether (EO addition number 25, hydroxyl value 53 mgKOH / g), add 1.5g of urea, start stirring, and then add 16.5g of aminosulfonic acid and mix evenly (molar ratio of aminosulfonic acid to octadecylamine polyoxyethylene ether terminal hydroxyl group is 1.8:1). Heat to 130℃ and react for 4.5h until the hydroxyl conversion rate of the reaction system is ≥92%, to obtain octadecylamine polyoxyethylene ether sulfonate. S2. After cooling the reaction system to 70°C, add ethylene glycol methyl ether (15% of the leveling agent), then add deionized water for dilution, and adjust the pH to 7.0 with triethanolamine to obtain a yellow, transparent, viscous liquid with a solid content of about 40%, which is octadecylamine polyoxyethylene ether sulfonate leveling agent.

[0023] Comparative Example 1 This comparative example provides a method for preparing a fatty amine polyoxyethylene ether sulfonate leveling agent, comprising adding ethylene glycol methyl ether (containing 15% of the leveling agent) to octadecylamine polyoxyethylene ether (EO addition number of 25, hydroxyl value of 53 mg KOH / g), then adding deionized water for dilution, adjusting the pH to 7.0 with triethanolamine, and obtaining a yellow transparent viscous liquid with a solid content of approximately 40%, which is the octadecylamine polyoxyethylene ether leveling agent.

[0024] Comparative Example 2 This comparative example provides a method for preparing a fatty amine polyoxyethylene ether sulfonate leveling agent, comprising the following steps: S1. Take 100g of octadecylamine polyoxyethylene ether (EO addition number is 25, hydroxyl value is 53mgKOH / g), add sulfuric acid to neutralize to neutral, then add 2.5g of urea, start stirring, then add 17.4g of aminosulfonic acid and mix evenly (molar ratio of aminosulfonic acid to octadecylamine polyoxyethylene ether terminal hydroxyl group is 1.9:1), heat to 130℃ and react for 4.5h until the hydroxyl conversion rate of the reaction system is ≥92%, to obtain octadecylamine polyoxyethylene ether sulfonate; S2. After cooling the reaction system to 70°C, add ethylene glycol methyl ether (15% of the leveling agent), then add deionized water for dilution, and adjust the pH to 7.0 with triethanolamine to obtain a yellow, transparent, viscous liquid with a solid content of about 40%, which is octadecylamine polyoxyethylene ether sulfonate leveling agent.

[0025] Application Example 1 This application example provides a method for preparing a fatty amine polyoxyethylene ether sulfonate leveling agent. The fatty amine polyoxyethylene ether sulfonate leveling agent prepared by this method is used in the dyeing and fixing process of nylon fabrics. The method includes: placing the nylon fabric in a dye bath at room temperature with a bath ratio of 1:20, then adding the octadecylamine polyoxyethylene ether sulfonate leveling agent prepared in Example 1 (at a dosage of 2% owf). After the dye is evenly dispersed, acid dyes (NHF-S type Acid Blue and Acid Yellow at a mass ratio of 1:1, at a dosage of 2% owf) are added. The pH of the dye bath is adjusted to 4.5, and the temperature is increased to 80°C at a rate of 2°C / min. Then, a bisphenol type fixing agent (bisphenol S type, at a dosage of 3% owf) is slowly added over a period of 30 min. After the acid fixing agent is added, the temperature is increased to 98°C at a rate of 2°C / min and held for 30 min. Finally, the temperature is lowered to 45°C, the dye is drained, washed with water, and dehydrated.

[0026] Application Example 2 The difference between this application example and application example 1 is that the fatty amine polyoxyethylene ether sulfonate leveling agent prepared in example 2 is used, while the rest are the same as in application example 1.

[0027] Application Example 3 The difference between this application example and application example 1 is that the fatty amine polyoxyethylene ether sulfonate leveling agent prepared in example 3 is used, while the rest are the same as in application example 1.

[0028] Application Example 4 The difference between this application example and application example 1 is that the liquor ratio is 1:10, the amount of dye used is 2% owf, the amount of octadecylamine polyoxyethylene ether sulfonate leveling agent is 3.0% owf, and the amount of the acidic fixing agent is 3% owf. All other aspects are the same as in application example 1.

[0029] Application Example 5 The difference between this application example and application example 1 is that the liquor ratio is 1:20, the amount of dye used is 2.0% owf, the amount of octadecylamine polyoxyethylene ether sulfonate leveling agent used is 2.0% owf, and the amount of acid fixing agent used is 2.0% owf. All other aspects are the same as in application example 1.

[0030] Application Example 6 The difference between this application example and application example 1 is that the acidic fixing agent is a high molecular weight copolymer resin, while the rest are the same as in application example 1.

[0031] Comparative Application Example 1 The difference between this application example and application example 1 is that the fatty amine polyoxyethylene ether leveling agent prepared in comparative example 1 is used, while the rest are the same as in application example 1.

[0032] Comparative Application Example 2 The difference between this application example and application example 1 is that the fatty amine polyoxyethylene ether leveling agent prepared in comparative example 2 is used, while the rest are the same as in application example 1.

[0033] Comparative Application Example 3 The difference between this application example and application example 1 is that no leveling agent is added; otherwise, they are the same as application example 1.

[0034] During the dyeing and fixing process in Application Examples 1-6 and Comparative Application Examples 1-3, we observed whether there was any sticking to the wall or flocculation and precipitation of the working solution. At the same time, we conducted tests on the levelness, migration rate and wash fastness of the nylon fabrics after the dyeable fixing process. The test methods are as follows, and the test results are shown in Table 1.

[0035] Evenness dyeing: Test the color difference (CMC ΔE) at multiple points on the same nylon fabric. The smaller the ΔE value, the better the evenness dyeing.

[0036] Dye transfer rate: The dyed and fixed nylon fabric and nylon white cloth were tested according to the conventional dye transfer process (liquor ratio 1:20, 98℃, 30min), and the dyeing degree (%) of the nylon white cloth was measured. The higher the value, the stronger the dye transfer ability.

[0037] Wash fastness: After washing, the staining of multi-fiber strips is judged and graded.

[0038] Table 1 Performance test results of the examples and comparative examples

[0039] As can be seen from the test results in Table 1, compared with comparative application examples 1-3, the fatty amine polyoxyethylene ether sulfonate leveling agent prepared by the method of the present invention can achieve better same-bath stability when applied to the dyeing and fixing process of nylon fabrics, and the leveling performance and fixing performance are also superior.

[0040] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to preferred embodiments, it is not limited to those listed in the embodiments. Those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A method for preparing a fatty amine polyoxyethylene ether sulfonate leveling agent, characterized in that, include: S1. Vacuum dehydration treatment of fatty amine polyoxyethylene ether is carried out, and then urea and aminosulfonic acid are added in sequence and mixed evenly. The reaction is carried out at a temperature until the hydroxyl conversion rate of the reaction system is ≥92% to obtain fatty amine polyoxyethylene ether sulfonate. S2. After cooling the reaction system, add an organic solvent, then add deionized water for dilution, and adjust the pH to 6.5~7.5 to obtain a fatty amine polyoxyethylene ether sulfonate leveling agent. The hydroxyl value of the fatty amine polyoxyethylene ether is 52 mg KOH / g to 56 mg KOH / g, and the molar ratio of the aminosulfonic acid to the terminal hydroxyl group of the fatty amine polyoxyethylene ether is 1.8 to 2:

1.

2. The method for preparing the fatty amine polyoxyethylene ether sulfonate leveling agent according to claim 1, characterized in that, The mixture comprises, by weight, 100 parts of the fatty amine polyoxyethylene ether, 1.5 to 4.5 parts of the urea, and 16.5 to 19.5 parts of the aminosulfonic acid.

3. The method for preparing the fatty amine polyoxyethylene ether sulfonate leveling agent according to claim 1, characterized in that, The fatty amine polyoxyethylene ether has 12 to 18 carbon atoms and 10 to 25 polyoxyethylene additions.

4. The method for preparing the fatty amine polyoxyethylene ether sulfonate leveling agent according to claim 1, characterized in that, The vacuum dehydration process includes treatment for 0.5 to 3 hours under conditions of vacuum degree ≥ 0.09 MPa and temperature of 90℃ to 100℃.

5. The method for preparing the fatty amine polyoxyethylene ether sulfonate leveling agent according to claim 1, characterized in that, The heating reaction involves raising the system temperature to 125℃~135℃ and holding it at that temperature for 3.5h~5h.

6. The method for preparing the fatty amine polyoxyethylene ether sulfonate leveling agent according to claim 1, characterized in that, The substance used to adjust the pH is at least one of ammonia or triethanolamine.

7. The method for preparing the fatty amine polyoxyethylene ether sulfonate leveling agent according to claim 1, characterized in that, The solid content of the fatty amine polyoxyethylene ether sulfonate leveling agent is 30%~60%.

8. The application of a fatty amine polyoxyethylene ether sulfonate leveling agent prepared by the method according to any one of claims 1 to 7 in the dyeing and fixing of nylon fabrics in a single bath, characterized in that, include: At room temperature, place the nylon fabric in a dye bath, then add the fatty amine polyoxyethylene ether sulfonate leveling agent. After it is evenly dispersed, add the acid dye or metal complex dye, adjust the pH of the dye bath to 4.5~6.5, and raise the temperature to 75~85℃ at a rate of 1℃ / min~3℃ / min. Then slowly add the acid fixing agent over a period of 25min~35min. After the acid fixing agent is added, raise the temperature to 95~105℃ at a rate of 2℃ / min~3℃ / min and hold for 20min~40min. Finally, lower the temperature to 40℃~50℃, drain the solution, and wash with water.

9. The application according to claim 8, characterized in that, The liquor ratio for dyeing and fixing in the same bath is 1:8~20, the amount of dye used is 0.5~5.0% owf, the amount of fatty amine polyoxyethylene ether sulfonate leveling agent used is 0.5~3.0% owf, and the amount of acidic fixing agent used is 1.0~5.0% owf.

10. The application according to claim 8, characterized in that, The acidic fixing agent is selected from bisphenol-type fixing agents.

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