Efficient polyester color fixing agent as well as preparation method and application thereof

Abstract

The invention relates to the technical field of color fixing agents, in particular to an efficient polyester color fixing agent and a preparation method and application thereof. The efficient polyester color fixing agent is prepared from the following components in percentage by weight: 20 to 40 percent of quaternary ammonium salt type cationic polymer, 5 to 15 percent of cross-linking agent, 2 to 8 percent of ultraviolet absorbent, 2 to 8 percent of penetrant, 0.5 to 3 percent of pH regulator and the balance of deionized water, the cross-linking agent is a polyfunctional group epoxy compound. According to the efficient polyester color fixing agent, the color fastness, especially the color fastness to washing and the color fastness to rubbing, of dyed polyester is remarkably improved through the electrostatic interaction of the cationic polymer and dye molecules and a three-dimensional network structure formed by the cross-linking agent, an ultraviolet light absorber is introduced into the cationic polymer through grafting reaction, and the color fastness to washing and the color fastness to rubbing are remarkably improved. The light fastness is obviously improved; tests show that the color fastness to washing can reach grade 4-5, the color fastness to rubbing can reach grade 4 or above in dry friction, and the color fastness to rubbing can reach grade 3-4 in wet friction.

Description

Technical Field

[0001] The present invention relates to the technical field of color fixing agents, and in particular to a high-efficiency polyester color fixing agent and a preparation method and application thereof. Background Art

[0002] Polyester fibers are widely used in the textile industry due to their excellent properties, including good elasticity, high strength, crispness, wrinkle resistance, and quick-drying and washability. However, polyester fabrics are essentially polyester fibers, which, aside from two terminal hydroxyl groups, lack other polar groups. Consequently, they have very poor hydrophilicity and are prone to fading after dyeing. Therefore, during the polyester dyeing process, a fixing agent is added to improve the dye's fixation rate on the fiber and reduce fading during washing.

[0003] Common dye-fixing agents on the market work by forming a film on the fabric surface, as described in Chinese invention patent publication number CN104846675B. This film prevents the dye molecules from loosely binding to the polyester fabric and causing discoloration upon washing. However, this surface film formation affects the fabric's feel and color, and can also degrade fabric quality. Some dye-fixing agents also require complex and costly preparation processes, making them unsuitable for large-scale industrial production. Therefore, developing an efficient, environmentally friendly, minimally impactful polyester dye-fixing agent with a simple preparation process is of great practical significance. Summary of the Invention

[0004] The technical problem to be solved by the present invention is to provide a high-efficiency polyester color fixing agent with simple process and little influence on fabric properties, as well as a preparation method and application thereof.

[0005] In order to solve the above technical problems, the technical solution adopted by the present invention is as follows: a high-efficiency polyester fixing agent, comprising the following components by weight percentage: 20-40% of a quaternary ammonium salt cationic polymer, 5-15% of a cross-linking agent, 2-8% of an ultraviolet absorber, 2-8% of a penetrant, 0.5-3% of a pH regulator, and the balance of deionized water; The cross-linking agent is a multifunctional epoxy compound.

[0006] Another technical solution adopted by the present invention is: a method for preparing the above-mentioned high-efficiency polyester color fixing agent, comprising the following steps: adding a portion of deionized water to a quaternary ammonium salt cationic polymer, and after the quaternary ammonium salt cationic polymer is completely dissolved, adding a crosslinking agent and an ultraviolet light absorber to react; then adding the remaining deionized water, a penetrant, and a pH adjuster to obtain the high-efficiency polyester color fixing agent.

[0007] Another technical solution adopted by the present invention is: the use of the above-mentioned high-efficiency polyester fixing agent includes the following steps: washing and dehydrating the dyed polyester fabric in sequence, then immersing it in water containing 2-5g / L of the high-efficiency polyester fixing agent for treatment, and after treatment, taking out the polyester fabric and washing and drying it in sequence.

[0008] The beneficial effects of the present invention are as follows: the high-efficiency polyester color fixing agent of the present invention significantly improves the color fastness of the dyed polyester, especially the color fastness to washing and the color fastness to rubbing, through the electrostatic interaction between the cationic polymer and the dye molecules and the three-dimensional network structure formed by the crosslinking agent, and introduces the ultraviolet absorber into the cationic polymer through a grafting reaction, thereby significantly improving the light fastness; according to tests, the color fastness to washing can reach level 4 to 5, the color fastness to rubbing can reach above level 4 in dry rubbing, and can reach level 3 to 4 in wet rubbing. DETAILED DESCRIPTION

[0009] To explain the technical content, achieved objectives and effects of the present invention in detail, the following describes them in conjunction with the implementation methods.

[0010] A high-efficiency polyester color fixing agent, comprising the following components by weight: 20-40% of a quaternary ammonium salt cationic polymer, 5-15% of a cross-linking agent, 2-8% of an ultraviolet light absorber, 2-8% of a penetrant, 0.5-3% of a pH regulator, and the balance of deionized water; The cross-linking agent is a multifunctional epoxy compound.

[0011] As can be seen from the above description, the beneficial effects of the present invention are as follows: the high-efficiency polyester color fixing agent of the present invention includes a quaternary ammonium salt cationic polymer, a crosslinking agent, an ultraviolet light absorber, a penetrant, and a pH regulator. These ingredients have minimal impact on the feel and color of the fabric, do not cause problems such as fabric hardening and discoloration, and maintain the original excellent properties of the polyester fabric. When the cationic polymer, crosslinking agent, and ultraviolet light absorber are compounded, the color fixing effect and light resistance are enhanced through crosslinking and grafting reactions. The quaternary ammonium salt cationic polymer has good cationic properties and can bind to negatively charged dye molecules through electrostatic interaction, thereby improving the dye's fixation rate on the fiber. At the same time, the quaternary ammonium salt cationic polymer can undergo a crosslinking reaction with a multifunctional epoxy compound to form a three-dimensional network structure, further improving the color fixing effect. The penetrant can help the color fixing agent quickly penetrate into the fiber, improving the color fixing efficiency. The introduction of the ultraviolet light absorber into the cationic polymer through a grafting reaction can significantly improve the light fastness. The pH regulator can adjust the pH value of the color fixing agent solution to stabilize its performance.

[0012] Multifunctional epoxy compounds contain multiple epoxy groups within their molecules, giving them a higher crosslinking density and reactivity, forming a more complex three-dimensional network structure. This gives the fixing agent greater mechanical strength, heat resistance, and corrosion resistance, and allows it to more effectively form a strong crosslinking structure with fibers and dye molecules, significantly improving color fastness. The resulting film after curing is relatively hard, with excellent chemical and abrasion resistance.

[0013] The content of the quaternary ammonium salt cationic polymer in the present invention is 20-40wt%, which can ensure sufficient cationic active sites to bind to the fiber and dye, while also avoiding excessive viscosity or cost increases caused by excessive concentrations. At the same time, a ratio of 20-40wt% can provide good film-forming properties and flexibility, helping to improve the feel of the fabric. If the content of the crosslinking agent is too low, the crosslinking density is insufficient, which may lead to unstable color fixation; while if the content is too high, the color fixer may be too hard, affecting the feel of the fabric; therefore, the content is controlled to 5-15%. A moderate crosslinking density can be formed between the cationic polymers, thereby significantly improving the durability of the color fixer. The quaternary ammonium salt cationic polymer and crosslinking agent in an appropriate ratio can provide a crosslinked network with good flexibility and high strength.

[0014] If the proportion of penetrant is too low, the penetration effect is poor; if the proportion is too high, the stability of the fixing agent may be reduced, and even the hydrophilicity of the fabric may be affected. The present invention controls the proportion of penetrant to 2~8wt% to effectively reduce the surface tension of the fixing agent, making it easier for it to penetrate into the polyester fiber, ensuring that the fixing agent is in full contact with the fiber, making the dye and the fiber more firmly bonded, reducing the shedding of the dye in subsequent treatment, and reducing the burden of the fixing agent in removing floating color. After using the penetrant, the amount of the fixing agent can be appropriately reduced. 0.5~3wt% of the pH adjuster can ensure that the reaction is carried out within the optimal pH range and avoid the occurrence of side reactions. The formula of the present invention avoids the cost increase and performance degradation caused by excessive ingredients while ensuring the color fixing effect.

[0015] Furthermore, the multifunctional epoxy compound is trimethylolpropane triglycidyl ether.

[0016] Furthermore, the weight average molecular weight of the quaternary ammonium salt cationic polymer is 5,000 to 20,000.

[0017] Furthermore, the penetrant is fatty alcohol polyoxyethylene ether.

[0018] From the above description, it can be seen that the HLB value (hydrophile-lipophile balance) of fatty alcohol polyoxyethylene ether is 10~15, which has good penetration performance.

[0019] Furthermore, the pH regulator is citric acid or sodium dihydrogen phosphate.

[0020] Furthermore, the ultraviolet light absorber contains at least one of a hydroxyl group, a carboxyl group and an amino group.

[0021] From the above description, it can be seen that the hydroxyl group, an active group, can undergo esterification, etherification or grafting reactions with amino groups or epoxy groups in cationic polymers; salicylate UV absorbers contain carboxyl groups, which can be grafted with hydroxyl groups or amino groups in cationic polymers through esterification reactions; certain substituted acrylonitrile UV absorbers contain amino groups, which can react with carboxyl groups or epoxy groups in cationic polymers.

[0022] Furthermore, the ultraviolet light absorber is at least one of UV-9, UV-531 and UV-326.

[0023] From the above description, it can be seen that UV-9, UV-531 and UV-326 contain hydroxyl groups, which can undergo grafting reaction with cationic polymers.

[0024] Preferably, the ultraviolet light absorber is UV-9.

[0025] From the above description, it can be seen that the UV-9 molecule contains an active group, hydroxyl, which can undergo a grafting reaction with cationic polymers. At the same time, UV-9 has good compatibility with a variety of polymers (including cationic polymers), can be evenly dispersed in the polymer matrix, can absorb ultraviolet rays with a wavelength of 290~380nm, covering most of the ultraviolet band, has good light stability and thermal stability, is not easy to decompose during use, has low toxicity, and meets environmental protection and safety requirements.

[0026] Another technical solution adopted by the present invention is: a method for preparing the above-mentioned high-efficiency polyester color fixing agent, comprising the following steps: adding a portion of deionized water to a quaternary ammonium salt cationic polymer, and after the quaternary ammonium salt cationic polymer is completely dissolved, adding a crosslinking agent and an ultraviolet light absorber to react; then adding the remaining deionized water, a penetrant, and a pH adjuster to obtain the high-efficiency polyester color fixing agent.

[0027] As can be seen from the above description, the preparation method of the present invention has a simple process, mild reaction conditions, low raw material cost, and is suitable for large-scale industrial production.

[0028] The quaternary ammonium salt cationic polymer needs to be dissolved before it can fully react with other components. Therefore, adding the crosslinker and ultraviolet light absorber after the quaternary ammonium salt cationic polymer is completely dissolved can avoid problems such as uneven distribution of the ultraviolet light absorber, incomplete reaction, low grafting efficiency, etc., which affect the performance of the final color fixing agent.

[0029] The present invention prevents the cationic polymer from agglomerating by adding deionized water in batches, making it easier to dissolve. The dissolution rate can be better controlled to avoid solution instability or excessively high local concentration caused by excessive dissolution. The reaction temperature can also be better controlled to ensure the uniformity and stability of the reaction.

[0030] Furthermore, during the preparation of the high-efficiency polyester fixing agent, stirring is continued at a stirring speed of 200-300 r / min.

[0031] As can be seen from the above description, the present invention adopts a relatively fast stirring speed, which helps to accelerate the dissolution process, evenly disperse the components, and improve the reaction efficiency and uniformity. At the same time, the stirring speed should not be too fast, otherwise it is easy to generate bubbles and trigger side reactions.

[0032] Furthermore, the partial deionized water accounts for 85-95 wt % of the total deionized water.

[0033] Furthermore, the cross-linking agent and the ultraviolet light absorber are heated to 50-60° C. for reaction.

[0034] From the above description, it can be seen that the cross-linking reaction and the grafting reaction occur at 50-60°C. This relatively low temperature can avoid the influence of high temperature on the performance of the absorbent.

[0035] Further, the remaining deionized water was added and the temperature was lowered to 30-40° C., and then the osmotic agent and pH regulator were added.

[0036] Another technical solution adopted by the present invention is: the use of the above-mentioned high-efficiency polyester fixing agent includes the following steps: washing and dehydrating the dyed polyester fabric in sequence, then immersing it in water containing 2-5g / L of the high-efficiency polyester fixing agent for treatment, and after treatment, taking out the polyester fabric and washing and drying it in sequence.

[0037] As can be seen from the above description, the color fixing process of the present invention is simple to operate, uses a small amount of color fixing agent, can effectively reduce production costs and improve production efficiency.

[0038] Furthermore, the temperature of the water containing the high-efficiency polyester fixing agent is 50-60° C., the immersion time is 20-30 minutes, and the bath ratio is 1:10-1:20.

[0039] From the above description, it can be seen that heating can accelerate the chemical reaction between the fixing agent and the fiber and dye, making the fixing agent more effectively combined with the dye and fiber. Immersing in a heated state can make the dye molecules penetrate deeper into the fiber and form a stronger bond with the fiber, which reduces the shedding of the dye in subsequent use, thereby reducing dependence on the fixing agent.

[0040] Furthermore, the moisture content of the polyester fabric after dehydration is 60-80%.

[0041] From the above description, it can be seen that a moderate moisture content helps the fiber to fully swell, so that the dye and the fixing agent can be evenly dispersed and fully contacted, thereby improving the fixing effect.

[0042] Furthermore, water containing a high-efficiency polyester color fixing agent is used as a color fixing working solution, and the pH value of the color fixing working solution is adjusted to 5.5-7 with sodium dihydrogen phosphate before being immersed in the polyester fabric.

[0043] From the above description, we can see that Furthermore, the drying temperature is 80-100°C.

[0044] Embodiment 1 of the present invention is: A high-efficiency polyester fixing agent, composed of the following components, by weight percentage: 20% of a quaternary ammonium salt cationic polymer (polyquaternium-10 (JR-400) / Dow Chemical, USA) (weight-average molecular weight of 5000), 5% of trimethylolpropane triglycidyl ether, 2% of UV-9, 2% of fatty alcohol polyoxyethylene ether with an HLB value of 13, 3% of sodium dihydrogen phosphate, and the balance of deionized water.

[0045] The second embodiment of the present invention is a method for preparing a high-efficiency polyester fixing agent, comprising the following steps: S1: Add 500 g of deionized water into the reactor and start stirring at a speed of 250 r / min.

[0046] S2: Slowly add 300 g of a quaternary ammonium salt cationic polymer with a weight average molecular weight of 10,000 and stir for 45 minutes to completely dissolve it.

[0047] S3: Add 100 g of trimethylolpropane triglycidyl ether and 50 g of ultraviolet light absorber, raise the temperature to 55° C., and stir to react for 1.5 h.

[0048] S4: Add 50g of deionized water, cool to 35°C, add 50g of fatty alcohol polyoxyethylene ether with an HLB value of 12 and 5g of citric acid, stir evenly, and obtain a finished product of a high-efficiency polyester fixing agent.

[0049] The third embodiment of the present invention is the application of the high-efficiency polyester fixing agent prepared in the second embodiment, and the steps are as follows: Step 1: Wash and dehydrate the dyed polyester fabric until the moisture content is 70%.

[0050] Step 2: Prepare the color fixing working solution. Add the high-efficiency polyester color fixing agent prepared above into water at a dosage of 3 g / L, stir evenly, and adjust the pH value to 6 with citric acid.

[0051] Step 3: Immerse the polyester fabric in the color fixing solution with a bath ratio of 1:15 and treat at 55°C for 25 minutes.

[0052] Step 4: After treatment, take out the polyester fabric, wash it with water, and then dry it at 90℃.

[0053] In accordance with the requirements of GB / T 3921-2008 "Textiles — Tests for colour fastness — Colour fastness to washing with soap and soap", GB / T 3920-2008 "Textiles — Tests for colour fastness — Colour fastness to rubbing" and GB / T 8427-2019 "Textiles — Tests for colour fastness — Colour fastness to artificial light: Xenon arc fading lamp", the performance tests were carried out on the dried polyester fabric. The colour fastness to washing of the polyester fabric was level 4 to 5, the colour fastness to rubbing was level 4 for dry rubbing and level 3 to 4 for wet rubbing, and the colour fastness to sunlight was level 4. The fabric had a soft hand feel, bright color, and no obvious change.

[0054] Comparative Example 1 of the present invention is: The only difference between Comparative Example 1 and Example 1 is that a commercially available ordinary polyester color fixing agent (Yutao brand color fixing agent Y produced by Jinan Yutao Chemical Co., Ltd.) is used in an amount of 6 g / L.

[0055] The performance test of the polyester fabric after drying was carried out. The color fastness to washing of the polyester fabric was level 3 to 4, the color fastness to rubbing was level 3 for dry rubbing, level 2 to 3 for wet rubbing, and level 2 to 3 for sunlight. The fabric felt slightly harder and its color changed slightly.

[0056] The fourth embodiment of the present invention is a method for preparing a high-efficiency polyester fixing agent, comprising the following steps: S1: Add 400 g of deionized water into the reactor and start stirring at a speed of 200 r / min.

[0057] S2: Slowly add 400 g of a quaternary ammonium salt cationic polymer with a weight average molecular weight of 15,000 and stir for 60 minutes to completely dissolve it.

[0058] S3: Add 150 g of trimethylolpropane triglycidyl ether and 20 g of ultraviolet light absorber, raise the temperature to 60° C., and stir to react for 1 hour.

[0059] S4: Add 30g of deionized water, cool to 30°C, add 80g of fatty alcohol polyoxyethylene ether with an HLB value of 13 and 20g of sodium dihydrogen phosphate, stir evenly, and obtain a finished product of a high-efficiency polyester fixing agent.

[0060] The fifth embodiment of the present invention is the application of the high-efficiency polyester fixing agent prepared in the fourth embodiment, and the steps are as follows: Step 1: Wash and dehydrate the dyed polyester fabric until the moisture content is 60%.

[0061] Step 2: Prepare the color fixing working solution. Add the high-efficiency polyester color fixing agent prepared above into water at a dosage of 4 g / L, stir evenly, and adjust the pH value to 5.5 with sodium dihydrogen phosphate.

[0062] Step 3: Immerse the polyester fabric in the color fixing working solution with a bath ratio of 1:10 and treat at 60°C for 20 minutes.

[0063] Step 4: After treatment, take out the polyester fabric, wash it with water, and then dry it at 100℃.

[0064] The performance test of the polyester fabric after drying showed that the color fastness to washing was level 4 to 5, the color fastness to rubbing was level 4 to 5 for dry rubbing and level 4 for wet rubbing, and the color fastness to sunlight was level 4. The fabric had a soft hand feel, bright color, and no obvious changes.

[0065] The sixth embodiment of the present invention is a method for preparing a high-efficiency polyester fixing agent, comprising the following steps: S1: Add 600 g of deionized water into the reactor and start stirring at a speed of 300 r / min.

[0066] S2: Slowly add 200 g of a quaternary ammonium salt cationic polymer with a weight average molecular weight of 8000 and stir for 30 minutes to completely dissolve it.

[0067] S3: Add 50 g of trimethylolpropane triglycidyl ether and 80 g of ultraviolet light absorber, raise the temperature to 50° C., and stir to react for 2 h.

[0068] S4: Add 70g of deionized water, cool to 40°C, add 20g of fatty alcohol polyoxyethylene ether with an HLB value of 10 and 30g of citric acid, stir evenly, and obtain a finished product of a high-efficiency polyester fixing agent.

[0069] The seventh embodiment of the present invention is the application of the high-efficiency polyester fixing agent prepared in the sixth embodiment, and the steps are as follows: Step 1: Wash and dehydrate the dyed polyester fabric until the moisture content is 80%.

[0070] Step 2: Prepare the color fixing working solution. Add 2 g / L of the high-efficiency polyester color fixing agent prepared above into water, stir evenly, and adjust the pH value to 7 with citric acid.

[0071] Step 3: Immerse the polyester fabric in the color fixing working solution with a bath ratio of 1:20 and treat at 50°C for 30 minutes.

[0072] Step 4: After treatment, take out the polyester fabric, wash it with water, and then dry it at 80℃.

[0073] The performance test of the polyester fabric after drying showed that the color fastness to washing was level 4, the color fastness to rubbing was level 4 for dry rubbing and level 3 for wet rubbing, and the color fastness to sunlight was level 3-4. The fabric had a soft hand feel, bright color, and no obvious changes.

[0074] In summary, the high-efficiency polyester color fixing agent provided by the present invention, as well as its preparation method and application, have the following advantages: 1. Compounding cationic polymers, crosslinking agents and ultraviolet absorbers enhances the color fixing effect and light resistance through crosslinking and grafting reactions. This high-efficiency polyester color fixing agent has minimal effect on the feel and color of the fabric.

[0075] 2. The preparation method is simple, the reaction conditions are mild, the cost of raw materials is low, and it is suitable for large-scale industrial production.

[0076] 3. It is easy to operate and requires less fixing agent, which can effectively reduce production costs and improve production efficiency.

[0077] The above descriptions are merely embodiments of the present invention and are not intended to limit the patent scope of the present invention. Any equivalent transformations made using the description of the present invention, or directly or indirectly applied in related technical fields, are also included in the patent protection scope of the present invention.

Claims

1. A high-efficiency polyester fixing agent, characterized in that: The invention comprises the following components by weight percentage: 20-40% of quaternary ammonium salt cationic polymer, 5-15% of cross-linking agent, 2-8% of ultraviolet light absorber, 2-8% of penetrant, 0.5-3% of pH regulator and the balance of deionized water; The cross-linking agent is a multifunctional epoxy compound.

2. The high-efficiency polyester fixing agent according to claim 1, characterized in that: The weight average molecular weight of the quaternary ammonium salt cationic polymer is 5000-20000.

3. The high-efficiency polyester fixing agent according to claim 1, characterized in that: The penetrant is fatty alcohol polyoxyethylene ether.

4. The high-efficiency polyester fixing agent according to claim 1, characterized in that The pH regulator is citric acid or sodium dihydrogen phosphate.

5. The high-efficiency polyester fixing agent according to claim 1, characterized in that: The ultraviolet light absorber contains at least one group selected from the group consisting of a hydroxyl group, a carboxyl group and an amino group.

6. The method for preparing a high-efficiency polyester fixing agent according to any one of claims 1 to 5, characterized in that: The method comprises the following steps: adding part of deionized water to a quaternary ammonium salt cationic polymer, adding a crosslinking agent and an ultraviolet light absorber to react after the quaternary ammonium salt cationic polymer is completely dissolved; and then adding the remaining deionized water, a penetrant and a pH regulator to obtain a high-efficiency polyester color fixing agent.

7. The method for preparing a high-efficiency polyester fixing agent according to claim 6, characterized in that: After adding the cross-linking agent and the ultraviolet light absorber, the temperature is raised to 50-60° C. to carry out the reaction.

8. The method for preparing a high-efficiency polyester fixing agent according to claim 6, characterized in that: After adding the remaining deionized water, the temperature is lowered to 30-40° C., and then the osmotic agent and pH regulator are added.

9. The use of the high-efficiency polyester fixing agent according to any one of claims 1 to 5, characterized in that: The method comprises the following steps: sequentially washing and dehydrating the dyed polyester fabric, then immersing the dyed polyester fabric in water containing 2-5 g / L of the high-efficiency polyester color fixing agent for treatment, and after treatment, taking out the polyester fabric and sequentially washing and drying the dyed polyester fabric.

10. The use of the high-efficiency polyester fixing agent according to claim 9, characterized in that: The moisture content of the polyester fabric after dehydration is 60-80%.