Quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent, and preparation method and application thereof

Abstract

This invention belongs to the field of dyeing and printing auxiliaries technology, specifically relating to a quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent, its preparation method, and its application. The preparation method of the quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent of this invention includes the following steps: 1) preparing bi-carboxyl-terminated polyethylene glycol using succinic anhydride and polyethylene glycol; 2) adding adipic acid, hexamethylenediamine, and sodium hypophosphite as a catalyst to the bi-carboxyl-terminated polyethylene glycol, and carrying out a polycondensation reaction at elevated temperature; 3) preparing the quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent using the reaction product obtained in step 2). This invention also provides the application of the quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent in the fabric finishing process. The finishing agent of this invention can improve the hydrophilicity of nylon fiber fabrics.

Description

Technical Field

[0001] This invention belongs to the field of dyeing and printing auxiliaries technology, specifically relating to a quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent, its preparation method, and its application. Background Technology

[0002] Nylon fiber is the second largest synthetic fiber, second only to polyester in annual production and market application. Nylon fiber possesses excellent mechanical properties such as abrasion resistance, tensile strength, and resilience, while also boasting advantages like softness, delicate feel, and lightweight. In the apparel industry, it is commonly used to make sports underwear, socks, outdoor clothing, and functional outerwear. However, under standard conditions, the moisture absorption rate of nylon fiber is only about 4.5%. Although relatively hydrophilic amide bonds exist in the molecular chain of nylon fiber, the polyamide molecular chain is closed due to the good planarity of the amide groups and the strong intermolecular forces that make it prone to crystallization, preventing sufficient contact with external water molecules, resulting in poor hydrophilicity. Because the fiber has difficulty absorbing and conducting sweat excreted from the skin, it causes a noticeable feeling of stuffiness and dampness. Simultaneously, the low moisture absorption rate makes the fiber surface prone to the accumulation of static charge, leading to static electricity. These problems significantly limit the application of nylon fiber in fields requiring high hydrophilicity and wearing comfort. Therefore, improving the hydrophilicity of nylon fiber fabrics has become a research hotspot in the development of comfortable nylon fabrics.

[0003] Treating nylon fiber fabrics with hydrophilic finishing agents is currently the simplest, most efficient, and economical method. Commonly used hydrophilic finishing agents on the market include polyurethanes, polyester polyethers, polyether-modified polysiloxanes, polyamines, and polyamide polyethers. While these agents are suitable for nylon fiber fabrics, they often suffer from insufficient hydrophilicity or wash resistance, or yellowing. Therefore, there is a need to develop a dedicated hydrophilic finishing agent for nylon fiber fabrics that offers excellent overall performance in terms of hydrophilicity and wash resistance. Summary of the Invention

[0004] The technical problem to be solved by the present invention is to provide a quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent with good hydrophilicity and water wash resistance, as well as its preparation method and application.

[0005] To address the aforementioned technical problems, this invention provides a method for preparing a quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent, comprising the following steps: 1) Using succinic anhydride and polyethylene glycol, double-carboxyl-terminated polyethylene glycol was prepared; 2) Add adipic acid, hexamethylenediamine, and sodium hypophosphite as a catalyst to double-carboxyl-terminated polyethylene glycol, and raise the temperature to carry out a polycondensation reaction; 3) Prepare a quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent using the reaction product obtained in step 2).

[0006] As an improvement to the preparation method of the quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent of the present invention, the following steps are performed sequentially: 1) Under an inert gas atmosphere (including N2), succinic anhydride and phosphorous acid as a catalyst were added to molten polyethylene glycol, and the temperature was raised to 120±10℃ for esterification reaction for 2±0.2h. Then, after vacuuming, the reaction was kept at 120±10℃ for 20±2min to obtain double-carboxyl-terminated polyethylene glycol. The molar ratio of succinic anhydride to polyethylene glycol is (2±0.1):1; the amount of phosphorous acid added is 1.8~2.2 wt% (preferably 2 wt%) of the total mass of succinic anhydride and polyethylene glycol. 2) In an inert gas atmosphere (including N2), add adipic acid, hexamethylenediamine and sodium hypophosphite as a catalyst to the double-carboxyl-terminated polyethylene glycol obtained in step 1), and heat to 210~250℃ (preferably 240℃) to carry out polycondensation reaction for 1.5~3.5h (preferably 2.5h). The molar ratio of adipic acid: hexamethylenediamine: polyethylene glycol in step 1) is 0.6:(1.6~2):1; the amount of sodium hypophosphite catalyst added is 1.8~2.2 wt% (preferably 2 wt%) of the total mass of bicarboxyl-terminated polyethylene glycol, adipic acid and hexamethylenediamine. 3) After the reaction product (polyamide polyether copolymer, polyamide polyether finishing agent) obtained in step 2) is cooled to 60±10℃, a solvent is added and mixed evenly. Then, 2,3-epoxypropyltrimethylammonium chloride is added, and the temperature is raised to 80±10℃ to carry out a ring-opening addition reaction for 2±0.2h. After the reaction is completed, the solvent is removed by rotary evaporation to obtain the quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent. 2,3-Epoxypropyltrimethylammonium chloride: The molar ratio of polyethylene glycol in step 1) is (0.4 ± 0.05): 1; the amount of solvent added is 55-65% (preferably 60%) of the total mass of the reaction product (polyamide polyether copolymer) obtained in step 2) and 2,3-epoxypropyltrimethylammonium chloride.

[0007] As a further improvement to the preparation method of the quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent of the present invention: the number average molecular weight of polyethylene glycol is 800.

[0008] As a further improvement to the preparation method of the quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent of the present invention: Steps 1) to 3) are carried out under stirring conditions, with the stirrer speed being 300~360 rpm.

[0009] The heating rate for steps 1) to 3) is 1 to 2 °C / min.

[0010] As a further improvement to the preparation method of the quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent of the present invention: The solvent in step 3) is isopropanol.

[0011] As a further improvement to the preparation method of the quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent of the present invention, the following is preferred: The molar ratio of adipic acid: hexamethylenediamine: polyethylene glycol in step 1) is 0.6:1.8:1.

[0012] The present invention also provides a quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent prepared by any of the above methods.

[0013] This invention also provides the application of quaternary ammonium salt-based polyamide polyether hydrophilic finishing agents in the fabric finishing process.

[0014] The reaction process of the preparation method of the present invention is as follows:

[0015]

[0016]

[0017] The preparation method of this invention involves first preparing bicarboxyl-terminated polyethylene glycol by transesterification of succinic anhydride and polyethylene glycol, then adding adipic acid and hexamethylenediamine to prepare a polyamide-polyether copolymer via an amidation reaction. Finally, 2,3-epoxypropyltrimethylammonium chloride and isopropanol solvent are added, and a ring-opening addition reaction is performed to prepare a quaternary ammonium salt-based polyamide-polyether hydrophilic finishing agent containing cationic groups, polyamide segments, and polyether segments in its molecular structure. The preparation method of this invention is simple, the reaction conditions are mild, the cost is low, and the reproducibility is good. It has good development prospects for improving the hydrophilicity of nylon fiber fabrics. When this finishing agent is applied to nylon fiber fabrics, the polyether segments in the finishing agent molecule impart hydrophilicity to the finished fabric, the cationic groups can enhance the hydrophilicity of the finished fabric, and the polyamide segments have a similar molecular structure to nylon fibers. During high-temperature heat treatment (baking), they can undergo eutectic reaction with nylon fiber molecules, imparting hydrophilicity to the finished nylon fiber fabric and exhibiting good wash resistance.

[0018] The structural formula of the quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent is:

[0019] In the formula, a = 2~4; n = 15~20.

[0020] The number average molecular weight range of quaternary ammonium salt-based polyamide polyether hydrophilic finishing agents is 2300~3600.

[0021] By treating fabrics with quaternary ammonium salt-based polyamide polyether hydrophilic finishing agents that have good hydrophilicity, nylon fiber fabrics can be endowed with good hydrophilicity and wash resistance; specifically as follows: A finishing solution (30 g / L) was prepared by adding water to a quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent. The nylon fabric to be finished was immersed in the finishing solution and padded (pickup rate 89%). After padding, the fabric was dried (80℃, 5 min) and baked (170℃, 50 s) to complete the finishing of the nylon fabric.

[0022] This invention imparts a certain degree of hydrophilicity to nylon fiber fabrics by hydrogen bonding between polyether and water in the polyamide polyether hydrophilic finishing agent molecule; and further enhances the hydrophilicity of the nylon fiber fabrics by the ionization of water with the quaternary ammonium salt cationic groups.

[0023] The hydrophilic finishing agent (quaternary ammonium salt-based polyamide-polyether hydrophilic finishing agent) prepared in this invention contains cationic groups, polyamide segments, and polyether segments in its molecular structure. When applied to nylon fiber fabrics, the polyether segments in the finishing agent molecule impart hydrophilicity to the finished fabric, while the cationic groups enhance this hydrophilicity. The polyamide segments have a similar molecular structure to the nylon fiber fabric itself, and during high-temperature baking, they can undergo eutectic reaction with the nylon fiber molecules, imparting good water resistance to the finished fabric. The preparation method of this invention is simple, the reaction conditions are mild, the cost is low, and the reproducibility is good. It has promising development prospects for improving the hydrophilicity of nylon fiber fabrics.

[0024] Compared with the prior art, the present invention has the following beneficial effects: 1) In the quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent of the present invention, the polyether segments, due to the large number of polyoxyethylene units within their molecules, can form hydrogen bonds with water molecules, providing good hydrophilicity for the finished fabric; at the same time, the 2,3-epoxypropyltrimethylammonium chloride cationic groups introduced into the molecular structure can enhance the hydrophilicity of the finishing agent. Compared with the original nylon fiber fabric (capillary effect 3.7 cm / 5 min), the capillary effect of the nylon fiber fabric treated with the quaternary ammonium salt-based polyamide polyether finishing agent can be significantly improved, thereby enhancing the hydrophilicity of the finished nylon fiber fabric.

[0025] 2) The polyamide segments in the quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent of this invention have similarity to the molecular structure of nylon fiber fabric itself. During high-temperature baking, they can undergo eutectic reaction with nylon fiber molecules, giving the fabric good wash resistance. After 10 household washes, the wicking retention rate of the fabric is approximately 91%.

[0026] 3) The preparation method of the present invention is simple, the reaction conditions are mild, the cost is low, and the reproducibility is good.

[0027] In summary, the preparation method of the present invention utilizes the introduction of 2,3-epoxypropyltrimethylammonium chloride cationic groups to react with polyamide polyether segments via a ring-opening addition reaction to obtain a quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent, thereby enabling nylon fiber fabrics to acquire good hydrophilicity and washability; moreover, the preparation method is simple, the reaction conditions are mild, the cost is low, and the reproducibility is good. Attached Figure Description

[0028] The specific embodiments of the present invention will be further described in detail below with reference to the accompanying drawings.

[0029] Figure 1 The infrared spectrum of the No. 3 quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent prepared in Example 1; Figure 2 The dynamic wetting process of nylon fiber fabrics before and after treatment with the No. 3 finishing agent prepared in Example 1. Detailed Implementation

[0030] The present invention will be further described below with reference to specific embodiments, but the scope of protection of the present invention is not limited thereto: In the following embodiments: The mixer speed for steps 1) to 3) is 300-360 rpm. The heating rate of the oil bath in steps 1) to 3) is 1~2℃ / min.

[0031] Example 1: A method for preparing a quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent (considering the amount of hexamethylenediamine used): 1) Under a N2 atmosphere, 0.02 mol of polyethylene glycol-800 was fully melted at 60°C, and then 0.04 mol of succinic anhydride and phosphorous acid as a catalyst were added. The amount of phosphorous acid added was 2 wt% of the total mass of succinic anhydride and polyethylene glycol. The reaction was carried out at 120°C for 2 h under stirring. Then, the reaction was carried out at 120°C for 20 min under vacuum (-0.08~-0.095 MPa) with stirring to remove the water generated in the reaction and obtain double-carboxyl-terminated polyethylene glycol.

[0032] 2) Under a N2 atmosphere, 0.012 mol of adipic acid, different molar amounts (0.032 mol, 0.034 mol, 0.036 mol, 0.038 mol, and 0.04 mol) of hexamethylenediamine and sodium hypophosphite as a catalyst were added to the bicarboxyl-terminated polyethylene glycol obtained in step 1). The amount of sodium hypophosphite added was 2 wt% of the total mass of bicarboxyl-terminated polyethylene glycol, adipic acid, and hexamethylenediamine. Under stirring, the mixture was heated to 240°C and subjected to a polycondensation reaction for 2.5 h. The resulting product was named a polyamide-polyether copolymer.

[0033] 3) After the polyamide polyether copolymer obtained in step 2) is naturally cooled to 60°C, isopropanol is added as a solvent and stirred evenly. Then, 0.008 mol of 2,3-epoxypropyltrimethylammonium chloride is added, and the mixture is heated to 80°C under stirring to carry out a ring-opening addition reaction for 2 hours. After the reaction is completed, the isopropanol solvent is removed by vacuum rotary evaporation (at a temperature of 50°C) to obtain five kinds of quaternary ammonium salt-based polyamide polyether hydrophilic finishing agents, which are designated as finishing agents 1#, 2#, 3#, 4#, and 5#, respectively.

[0034] The amount of isopropanol used is 60% of the total mass of the polyamide polyether copolymer and 2,3-epoxypropyltrimethylammonium chloride.

[0035] When the amount of hexamethylenediamine used was 0.032 mol, the resulting product was named No. 1 finishing agent; When the amount of hexamethylenediamine used was 0.034 mol, the resulting product was named No. 2 finishing agent; When the amount of hexamethylenediamine used was 0.036 mol, the resulting product was named No. 3 finishing agent; When the amount of hexamethylenediamine used was 0.038 mol, the resulting product was named No. 4 finishing agent; When the amount of hexamethylenediamine used is 0.04 mol, the resulting product is named No. 5 finishing agent.

[0036] The infrared spectrum of finishing agent #3 in Example 1 is as follows: Figure 1 As shown. From Figure 1 It can be seen from the figure that he is 1695cm tall. -1 and 1545cm -1 The peaks at 2870 cm⁻¹ represent the stretching vibration peaks of C=O and NH in the amide bond (-CONH-), respectively. -1 The peak at 1097 cm⁻¹ represents the symmetric stretching vibration of -CH₂ in polyamide and -CH₃ in cation. -1 The peak at 954 cm⁻¹ represents the stretching vibration of COC in the polyether segment. -1 The peak at this location represents the bending vibration of CN in the cation. In summary, the finishing agent macromolecular chain contains polyamide segments, polyether segments, and cationic groups.

[0037] Experiment 1: The five finishing agents prepared in Example 1 were respectively diluted with water to prepare 30g / L finishing solutions. Nylon fiber fabrics were immersed in the finishing solutions. The nylon fiber fabrics were treated at room temperature by a one-dip two-ply method (total rinsing rate of 89%), then dried at 80℃ for 5min and baked at 170℃ for 50s to obtain five kinds of finished nylon fiber fabrics, which were designated as 1#, 2#, 3#, 4# and 5# finished fabrics, respectively. The untreated original fabric was designated as 0#.

[0038] To investigate the effect of different hexammonium diamine dosages of quaternary ammonium salt-based polyamide polyether hydrophilic finishing agents on the hydrophilicity of finished fabrics, the capillary effect of the fabrics was tested according to FZ / T01071-2008 "Textile Capillary Effect Test Method". The finished fabrics were washed according to standard GB / TT8629-2001 "Textile Testing - Household Washing and Drying Procedures". The capillary effect of the above five different finished fabrics was tested, and the results are shown in Table 1.

[0039] Table 1. Effects of quaternary ammonium salt-based polyamide polyether hydrophilic finishing agents prepared with different hexamethylenediamine dosages on the hydrophilicity and wash resistance of nylon fiber fabrics.

[0040] Table 1 shows that the hydrophilicity of all five treated fabrics was improved to varying degrees compared to the original fabric #0. When the amount of hexamethylenediamine (HDMA) was low, fewer polyamide segments were synthesized, resulting in poor wash resistance and fewer terminal amino groups that could undergo ring-opening addition reactions, leading to poor hydrophilic finishing. When the amount of HDMA was high, the number of terminal amino groups that could undergo ring-opening addition reactions increased, but the excessive addition of HDMA created a strongly alkaline environment. Under these conditions, the cationic groups accelerated hydrolysis, resulting in a slight decrease in the hydrophilicity of the treated fabric. Therefore, the optimal amount of HDMA was 0.036 mol.

[0041] Additionally, such as Figure 2 The following is stated: The instantaneous water contact angles of 0# (original fabric) at room temperature are 92.8°, 90.4°, and 86.5° at 0ms, 200ms, and 500ms, respectively. The wetting time of 0# (original fabric) at a water contact angle of 0° is 12500ms.

[0042] The instantaneous water contact angles of the No. 3 treated fabric at room temperature were 66.6° and 31.5° at 0 ms and 200 ms, respectively. The wetting time of the No. 3 treated fabric at a water contact angle of 0° was 470 ms.

[0043] After washing the No. 3 treated fabric ten times, the instantaneous water contact angles at room temperature at 0ms, 200ms, and 500ms were 69.8°, 53.5°, and 38.5°, respectively. The wetting time of the No. 3 treated fabric after washing ten times with a water contact angle of 0° was 1530ms.

[0044] Example 2: A method for preparing a quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent (considering the selection of polycondensation reaction temperature) 1) Equivalent to step 1) of Example 1. 2) Under a N2 atmosphere, 0.012 mol of adipic acid, 0.036 mol of hexamethylenediamine, and sodium hypophosphite as a catalyst were added to the bicarboxyl-terminated polyethylene glycol obtained in step 1). The amount of sodium hypophosphite added was 2 wt% of the total mass of the bicarboxyl-terminated polyethylene glycol, adipic acid, and hexamethylenediamine. Under stirring, the mixture was heated to different temperatures (210℃, 220℃, 230℃, 240℃, and 250℃, respectively) for polycondensation reaction for 2.5 h. The rest of the reaction was carried out as described in step 2) of Example 1. The resulting product was named polyamide polyether copolymer.

[0045] 3) Equivalent to step 3 of Example 1.

[0046] When the polycondensation reaction temperature is 210℃, the resulting product is named No. 6 finishing agent; When the polycondensation reaction temperature is 220℃, the resulting product is named No. 7 finishing agent; When the polycondensation reaction temperature is 230℃, the resulting product is named No. 8 finishing agent; When the polycondensation reaction temperature is 240°C, the resulting product is the No. 3 finishing agent in Example 1; When the polycondensation reaction temperature is 250℃, the resulting product is named No. 9 finishing agent.

[0047] Experiment 2: The finishing agent obtained in Example 2 was tested in accordance with the method described in Experiment 1 to investigate the hydrophilicity and wash resistance of fabrics treated with the quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent prepared at different polycondensation temperatures. The results are shown in Table 2.

[0048] Table 2. Effect of different polycondensation reaction temperatures on the hydrophilicity and wash resistance of fabrics treated with quaternary ammonium salt-based polyamide polyether hydrophilic finishing agents.

[0049] Table 2 shows that the hydrophilicity of all five treated fabrics was improved to varying degrees compared to the original fabric #0. As the reaction temperature increased, the hydrophilicity of the treated fabrics first increased and then decreased. This is because at lower reaction temperatures, the required activation energy cannot be provided, resulting in a slower reaction rate, less of the target product synthesized, and poor hydrophilicity. When the reaction temperature exceeds 240℃, it leads to the oxidation of polyether segments, exacerbating the thermal decomposition of the polyether segments and affecting the structure of the synthesized finishing agent, thus causing a decrease in hydrophilicity. Therefore, 240℃ was selected as the optimal reaction temperature.

[0050] Example 3: A method for preparing a quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent (considering the selection of polycondensation reaction time) 1) Equivalent to step 1) of Example 1. 2) Under N2 atmosphere, 0.012 mol adipic acid, 0.036 mol hexamethylenediamine and sodium hypophosphite as a catalyst were added to the bicarboxyl-terminated polyethylene glycol obtained in step 1). Under stirring, the temperature was raised to 240°C for different polycondensation reaction times (1.5 h, 2 h, 2.5 h, 3 h, and 3.5 h, respectively). The rest was the same as step 2 in Example 1. The resulting product was named polyamide polyether copolymer.

[0051] 3) Equivalent to step 3 of Example 1.

[0052] When the polycondensation reaction time is 1.5 h, the resulting product is named No. 10 finishing agent; When the polycondensation reaction time is 2 hours, the resulting product is named No. 11 finishing agent; When the polycondensation reaction time is 2.5 h, the resulting product is the No. 3 finishing agent in Example 1; When the polycondensation reaction time is 3 hours, the resulting product is named No. 12 finishing agent; When the polycondensation reaction time is 3.5 h, the resulting product is named No. 13 finishing agent.

[0053] Experiment 3: The finishing agent obtained in Example 3 was tested in accordance with the method described in Experiment 1 to investigate the hydrophilicity and wash resistance of fabrics treated with the quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent prepared with different polycondensation reaction times. The results are shown in Table 3.

[0054] Table 3 shows the effect of quaternary ammonium-based polyamide polyether hydrophilic finishing agents prepared at different polycondensation reaction times on the hydrophilic properties and wash resistance of fabrics treated with these agents.

[0055] Table 3 shows that the hydrophilicity of all five treated fabrics was improved to varying degrees compared to the original fabric #0. With increasing reaction time, the hydrophilicity of the treated fabrics initially increased and then tended to balance. This is because, as the reaction time increases, the polymer conversion rate gradually rises, leading to a gradual improvement in the hydrophilicity and wash resistance of the treated fabrics. However, if the reaction time is too long, the polyether will undergo oxidative decomposition at high temperatures, resulting in a decrease in the hydrophilicity and wash resistance of the treated fabrics. Therefore, 2.5 hours was selected as the optimal reaction time.

[0056] Comparative Example 1: In step 3) of Example 1, “2,3-epoxypropyltrimethylammonium chloride” was replaced with “3-chloro-2-hydroxypropyltrimethylammonium chloride”, while the molar amount remained unchanged, and the rest was the same as the preferred scheme of Example 1.

[0057] Comparative Experiment 1: The No. 3 finishing agent (N-PAPG) obtained in Example 1, the polyamide polyether copolymer obtained by step 2) of the No. 3 finishing agent in Example 1, the commercially available hydrophilic finishing agent, and the product obtained in Comparative Example 1 were used for hydrophilic finishing of nylon fiber fabrics. The results are shown in Table 4.

[0058] Table 4 Comparison of hydrophilic properties between self-made quaternary ammonium salt-based polyamide polyether water treatment agent (N-PAPG) and existing hydrophilic finishing agents

[0059] Commercially available hydrophilic finishing agent: Nylon hydrophilic finishing agent silicone oil SSN (Zhejiang Kefeng Organosilicon).

[0060] As can be seen from Table 4, compared with existing hydrophilic finishing agents, the quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent of the present invention has better hydrophilicity and water resistance. This is mainly because the presence of cationic groups in the finishing agent enhances the hydrophilicity of the finishing agent. At the same time, the finishing agent contains a polyamide structure, which will produce a eutectic effect with nylon fiber fabric during high-temperature baking, thereby improving the water resistance of the finished fabric.

[0061] Finally, it should be noted that the above examples are merely some specific embodiments of the present invention. Obviously, the present invention is not limited to the above embodiments and many variations are possible. All variations that can be directly derived or conceived by those skilled in the art from the disclosure of the present invention should be considered within the scope of protection of the present invention.

Claims

1. Process for the preparation of quaternary ammonium salt-based polyamide polyether hydrophilic finishing agents, characterized in that Includes the following steps: 1) Using succinic anhydride and polyethylene glycol, double-carboxyl-terminated polyethylene glycol was prepared; 2) Add adipic acid, hexamethylenediamine, and sodium hypophosphite as a catalyst to double-carboxyl-terminated polyethylene glycol, and raise the temperature to carry out a polycondensation reaction; 3) Prepare a quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent using the reaction product obtained in step 2).

2. The process for the preparation of quaternary ammonium salt based polyamide polyether hydrophilic finish according to claim 1, characterized in that Perform the following steps in sequence: 1) Under an inert gas atmosphere, succinic anhydride and phosphorous acid as a catalyst were added to molten polyethylene glycol, and the temperature was raised to 120±10℃ for esterification reaction for 2±0.2h. Then, after vacuuming, the reaction was kept at the temperature for 20±2min to obtain double-carboxyl-terminated polyethylene glycol. The molar ratio of succinic anhydride to polyethylene glycol is (2±0.1):1; the amount of phosphorous acid added is 1.8~2.2 wt% of the total mass of succinic anhydride and polyethylene glycol. 2) Under an inert gas atmosphere, add adipic acid, hexamethylenediamine and sodium hypophosphite as a catalyst to the double-carboxyl-terminated polyethylene glycol obtained in step 1), and heat to 210~250℃ to carry out polycondensation reaction for 1.5~3.5h. The molar ratio of adipic acid:hexamethylenediamine:polyethylene glycol in step 1) is 0.6:(1.6~2):1; the amount of sodium hypophosphite catalyst added is 1.8~2.2 wt% of the total mass of bicarboxyl-terminated polyethylene glycol, adipic acid, and hexamethylenediamine. 3) After the reaction product obtained in step 2) is cooled to 60±10℃, a solvent is added and mixed evenly. Then, 2,3-epoxypropyltrimethylammonium chloride is added and the temperature is raised to 80±10℃ to carry out a ring-opening addition reaction for 2±0.2h. After the reaction is completed, the solvent is removed by rotary evaporation to obtain a quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent. 2,3-Epoxypropyltrimethylammonium chloride: The molar ratio of polyethylene glycol in step 1) is (0.4 ± 0.05): 1; the amount of solvent added is 55-65% of the total mass of the reaction product obtained in step 2) and 2,3-epoxypropyltrimethylammonium chloride.

3. The preparation method of the quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent according to claim 2, characterized in that: The number average molecular weight of polyethylene glycol is 800.

4. The method for preparing the quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent according to claim 3, characterized in that: Steps 1) to 3) are carried out under stirring conditions, with a stirring speed of 300 to 360 rpm; The heating rate for steps 1) to 3) is 1 to 2 °C / min.

5. The method for preparing the quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent according to claim 4, characterized in that: The solvent in step 3) is isopropanol.

6. The process for the preparation of quaternary ammonium salt-based polyamide polyether hydrophilic finish according to any one of claims 2 to 5, characterized in that, Adipic acid: Hexamethylenediamine: polyethylene glycol in step 1) has a molar ratio of 0.6:1.8:

1.

7. A quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent prepared by any one of the methods described in claims 1 to 6.

8. The application of the quaternary ammonium salt-based polyamide polyether hydrophilic finishing agent as described in claim 7 in the fabric finishing process.

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