Cationic dyeing process based on polyamide-imide powder

Abstract

The application discloses a cationic dye dyeing method based on polyamide-imide powder, and specifically comprises the following steps: step 1, pretreatment of polyamide-imide powder; step 2, the polyamide-imide powder treated in step 1 is put into a dyeing solution for dyeing, and the dyed polyamide-imide powder is put into a soaping solution containing a washing powder solution for soaping to remove residual dyes and oil stains on the surface of the fabric; and the washed product is dried to obtain the final product. The application solves the problem of difficult dyeing of polyamide-imide powder and ensures the stability of the polyamide-imide structure.

Description

Technical Field

[0001] This invention belongs to the field of organic polymer material dyeing and finishing technology, and relates to a cationic dyeing method based on polyamide-imide powder. Background Technology

[0002] Polyamide-imide is a high-performance organic polymer material, a modified product of polyimide, possessing excellent heat resistance, corrosion resistance, high physical strength, and a low coefficient of friction. It remains stable at temperatures up to 350°C, making it suitable for various harsh environments. Due to its unique properties, it has been widely used in industrial and high-tech fields such as high-temperature filtration materials, wear-resistant coatings, and electronic packaging materials. As a high-performance material, its molecular structure is very compact and exhibits excellent stereoregularity. Because its powder itself has a golden-yellow hue and a high glass transition temperature (above approximately 300°C), it is difficult to dye under normal conditions.

[0003] Research on the staining of polyamide-imide materials is scarce, with most studies focusing on the staining process of polyimide materials themselves. Alkali pretreatment is an effective method for staining polyimide and has been extensively studied. Alkali treatment introduces anionic carboxyl groups onto the polyamide-imide surface, effectively increasing the dye number of cationic dyes on the polyamide-imide. However, alkali pretreatment increases the surface roughness of the sample, disrupting the original regular structure of the polyamide-imide and resulting in a significant loss of structural strength.

[0004] Carrier dyeing is a dyeing method that uses small molecule compounds as carriers, which have an affinity for both dyes and fibers. During the dyeing process, the carrier molecules enter the molecular chains of the target dye, breaking the intermolecular forces and increasing the intermolecular distance. This promotes the dye's penetration into the fiber, effectively increasing the dye uptake rate. Summary of the Invention

[0005] The purpose of this invention is to provide a cationic dyeing method based on polyamide-imide powder, which solves the problem of difficult dyeing of polyamide-imide powder and can ensure the stability of the polyamide-imide structure.

[0006] The technical solution adopted in this invention is a cationic dyeing method based on polyamide-imide powder, which specifically includes the following steps:

[0007] Step 1: Pretreatment of polyamide-imide powder;

[0008] Step 2: Place the polyamide-imide powder treated in Step 1 into the dye bath for dyeing. After dyeing, place the polyamide-imide powder into a soaping solution containing laundry detergent for soaping to remove residual dye and oil stains from the fabric surface. After washing, dry to obtain the final product.

[0009] The invention is further characterized by:

[0010] The specific process of step 1 is as follows: at room temperature, put the polyamide-imide powder into the soaping solution for soaping, and dry it after cleaning.

[0011] In step 1, the amount of polyamide-imide powder used is 1-20g, the concentration of laundry detergent in the soaping solution is 1-3g / L, the soaping temperature is 50-90℃, and the soaping time is 10-20min; the drying temperature is 60-80℃, and the drying time is 8-16h.

[0012] The specific process of step 2 is as follows:

[0013] Step 2.1: Add the polyamide-imide powder treated in step 1 into the dye bath, and heat it at a rate of 2℃ / min during the heating process. The dyeing temperature is 80-140℃, and then keep it at that temperature for 60min.

[0014] Step 2.2: Stop heating and continue stirring until the dye solution cools to room temperature. Then wash and dry the dyed polyamide-imide powder. Place the dyed polyamide-imide powder into the soaping solution for soaping and dry it after soaping.

[0015] In step 2.1, the preparation process of the dye solution is as follows:

[0016] Add cationic dye, purified water and benzyl alcohol to a beaker, adjust the pH of the solution to 3-6, stir well, and you will get the prepared dye solution.

[0017] In step 2.1, the mass ratio of polyamide-imide powder to dye solution is 1:15~30; the mass of cationic dye is 1-5% of the mass of polyamide-imide powder, and the concentration of benzyl alcohol is 10-60 g / L.

[0018] In step 2.2, the concentration of laundry detergent in the soaping solution is 1-3 g / L, the mass of the soaping solution is 30 times the mass of the powder used, the soaping temperature is 50-90℃, and the soaping time is 10-20 min.

[0019] In step 2.2, the drying temperature after staining is 80-120℃ and the drying time is 8-16 hours.

[0020] The beneficial effects of this invention are that the carrier-based dyeing method for polyamide-imide powder provided by this invention uses cationic red dye X-5GN and benzyl alcohol as a carrier to dye the polyamide-imide powder, thereby achieving low-temperature polyamide-imide dyeing. This method is simple to operate, requires minimal equipment, yields a high dyeing rate, has low reaction cost, excellent thermal properties, and good reaction effect. Attached Figure Description

[0021] Figure 1This is a flowchart of the dyeing process of the cationic dyeing method based on polyamide-imide powder according to the present invention;

[0022] Figure 2 This is an ultraviolet absorbance test of the residual dye solution after dyeing in Examples 1 to 6 of the present invention based on the cationic dye dyeing method of polyamide-imide powder;

[0023] Figure 3 This is an infrared test of a sample stained with cationic red dye and benzyl alcohol as a carrier in Example 6 of the cationic dye staining method based on polyamide-imide powder of the present invention, and an unstained sample.

[0024] Figure 4 This is the thermogravimetric analysis of the sample after staining with cationic red dye and benzyl alcohol as a carrier in Example 6 of the cationic dye staining method based on polyamide-imide powder of the present invention.

[0025] Figure 5 This is a UV absorbance test image of a black sample after dyeing using the cationic dye dyeing method based on polyamide-imide powder according to the present invention;

[0026] Figure 6 This is a UV absorbance test image of a brown sample after dyeing with the cationic dye method based on polyamide-imide powder according to the present invention.

[0027] Figure 7 This is a UV absorbance test image of a green sample after dyeing with the cationic dye method based on polyamide-imide powder according to the present invention;

[0028] Figure 8 This is a UV absorbance test image of a blue sample after dyeing with the cationic dye method based on polyamide-imide powder according to the present invention;

[0029] Figure 9 This is a UV absorbance test image of a purple sample after dyeing with a cationic dye based on polyamide-imide powder according to the present invention. Detailed Implementation

[0030] The present invention will now be described in detail with reference to the accompanying drawings and specific embodiments.

[0031] This invention relates to a cationic dyeing method based on polyamide-imide powder, which specifically includes the following steps:

[0032] Step 1, Pretreatment: At room temperature, the polyamide-imide powder is pretreated to wash and remove impurities;

[0033] Specifically, the polyamide-imide powder is placed in a soap solution containing laundry detergent and washed, then dried after washing.

[0034] In step 1, the amount of polyamide-imide powder used is 1-20g, the concentration of laundry detergent in the soaping solution is 1-3g / L, the mass of the soaping solution is 30 times the mass of the polyamide-imide powder used, the soaping temperature is 50-90℃, the soaping time is 10-20min; the drying temperature is 60-80℃, and the drying time is 8-16h.

[0035] Step 2, Dyeing: Add the cleaned and dried polyamide-imide powder to the prepared dye bath for dyeing. Increase the temperature at a rate of 2℃ / min, and the dyeing temperature is 80-140℃. Stir continuously and then keep warm for 60 minutes. Stop heating and continue stirring until it slowly cools to room temperature. After dyeing, put the dyed polyamide-imide powder into a soaping solution containing laundry detergent to wash it to remove residual dye and oil on the fabric surface. After washing, dry it. Dyeing is complete.

[0036] The mass ratio of polyamide-imide powder to the prepared dye solution is 1:15~30;

[0037] The specific preparation process of the dye solution is as follows: add a certain amount of cationic red dye, purified water and benzyl alcohol to a beaker to make the dye solution, then add acetic acid to adjust the pH value of the dye solution to 3~6, ​​and then stir the dye solution continuously for 30 minutes until it is evenly mixed.

[0038] The cationic dye is 1-5% of the mass of the polyamide-imide powder, and the benzyl alcohol concentration is 10-60 g / L.

[0039] The concentration of laundry detergent in the soaping solution is 1-3 g / L, the mass of the soaping solution is 30 times the mass of the powder used, the soaping temperature is 50-90℃, and the soaping time is 10-20 min; after the soaping is finished, the drying temperature is 80-120℃, and the drying time is 8-16 hours.

[0040] Example 1

[0041] This invention relates to a cationic dyeing method based on polyamide-imide powder, which specifically includes the following steps:

[0042] Step 1: Weigh 60g of purified water and 0.18g of laundry detergent at room temperature to prepare a soaping solution with a concentration of 3g / L. Add 2g of polyamide-imide powder to the soaping solution and soap for 15 minutes at a soaping temperature of 70℃. After soaping, dry in a hot air drying oven at 70℃ for 12 hours.

[0043] Step 2: Prepare the dye solution. Add 0.08g of cationic red dye, 40g of purified water, and 0.8g of benzyl alcohol to a beaker. Adjust the pH of the dye solution to 3-4 using acetic acid. Stir the dye solution continuously for 30 minutes to ensure uniformity. The dye solution is now ready. Mix the dried powder into the prepared dye solution, place the mixture in a constant temperature magnetic stirring oil bath with a magnetic stir bar, and slowly heat to 130℃. Maintain this temperature for 60 minutes while continuously stirring.

[0044] Step 3: Stop heating and continue stirring until it slowly cools to room temperature. Rinse and filter the polyamide-imide powder. Place the filtered polyamide-imide powder in a soap solution with the same components as in Step 1 for washing. After washing, dry in a hot air drying oven at 90°C for 12 hours.

[0045] Example 2

[0046] This invention relates to a cationic dyeing method based on polyamide-imide powder, which specifically includes the following steps:

[0047] Step 1: Weigh 60g of purified water and 0.18g of laundry detergent at room temperature to prepare a soaping solution with a concentration of 3g / L. Add 2g of polyamide-imide powder to the soaping solution and soap for 15 minutes at a soaping temperature of 70℃. After soaping, dry in a hot air drying oven at 70℃ for 12 hours.

[0048] Step 2: Prepare the dye solution. Add 0.08g of cationic red dye, 40g of purified water, and 1.2g of benzyl alcohol to a beaker. Adjust the pH of the dye solution to 3-4 using acetic acid. Stir the dye solution continuously for 30 minutes to ensure uniformity. The dye solution is now ready. Mix the dried powder into the prepared dye solution, place the mixture in a constant temperature magnetic stirring oil bath with a magnetic stir bar, and slowly heat to 130℃. Maintain this temperature for 60 minutes while continuously stirring.

[0049] Step 3: Stop heating and continue stirring until it slowly cools to room temperature. Rinse and filter the polyamide-imide powder. Place the filtered polyamide-imide powder in a soap solution with the same components as in Step 1 for washing. After washing, dry in a hot air drying oven at 90°C for 12 hours.

[0050] Example 3

[0051] This invention relates to a cationic dyeing method based on polyamide-imide powder, which specifically includes the following steps:

[0052] Step 1: Weigh 60g of purified water and 0.18g of laundry detergent at room temperature to prepare a soaping solution with a concentration of 3g / L. Add 2g of polyamide-imide powder to the soaping solution and soap for 15 minutes at a soaping temperature of 70℃. After soaping, dry in a hot air drying oven at 70℃ for 12 hours.

[0053] Step 2: Prepare the dye solution. Add 0.08g of cationic red dye, 40g of purified water, and 1.6g of benzyl alcohol to a beaker. Adjust the pH of the dye solution to 3-4 using acetic acid. Stir the dye solution continuously for 30 minutes to ensure uniformity. The dye solution is now ready. Mix the dried powder into the prepared dye solution, place the mixture in a constant temperature magnetic stirring oil bath with a magnetic stir bar, and slowly heat to 130℃. Maintain this temperature for 60 minutes while continuously stirring.

[0054] Step 3: Stop heating and continue stirring until it slowly cools to room temperature. Rinse and filter the polyamide-imide powder. Place the filtered polyamide-imide powder in a soap solution with the same components as in Step 1 for washing. After washing, dry in a hot air drying oven at 90°C for 12 hours.

[0055] Example 4

[0056] Step 1: Weigh 60g of purified water and 0.18g of laundry detergent at room temperature to prepare a soaping solution with a concentration of 3g / L. Add 2g of polyamide-imide powder to the soaping solution and soap for 15 minutes at a soaping temperature of 70℃. After soaping, dry in a hot air drying oven at 70℃ for 12 hours.

[0057] Step 2: Prepare the dye solution. Add 0.08g of cationic red dye, 40g of purified water, and 2g of benzyl alcohol to a beaker. Adjust the pH of the dye solution to 3-4 using acetic acid. Stir the dye solution continuously for 30 minutes to ensure uniformity. The dye solution is now ready. Mix the dried powder into the prepared dye solution, place the mixture in a constant temperature magnetic stirring oil bath with a magnetic stir bar, and slowly heat to 130℃. Maintain this temperature for 60 minutes while continuously stirring.

[0058] Step 3: Stop heating and continue stirring until it slowly cools to room temperature. Rinse and filter the polyamide-imide powder. Place the filtered polyamide-imide powder in a soap solution with the same components as in Step 1 for washing. After washing, dry in a hot air drying oven at 90°C for 12 hours.

[0059] Example 5

[0060] Step 1: Weigh 60g of purified water and 0.18g of laundry detergent at room temperature to prepare a soaping solution with a concentration of 3g / L. Add 2g of polyamide-imide powder to the soaping solution and soap for 15 minutes at a soaping temperature of 70℃. After soaping, dry in a hot air drying oven at 70℃ for 12 hours.

[0061] Step 2: Prepare the dye solution. Add 0.08g of cationic red dye, 40g of purified water, and 1.6g of benzyl alcohol to a beaker. Adjust the pH of the dye solution to 5-6 using acetic acid. Stir the dye solution continuously for 30 minutes to ensure uniformity. The dye solution is now ready. Mix the dried powder into the prepared dye solution, place the mixture in a thermostatic magnetic stirring oil bath with a magnetic stir bar, and slowly heat to 130℃. Maintain this temperature for 60 minutes while continuously stirring.

[0062] Step 3: Stop heating and continue stirring until it slowly cools to room temperature. Rinse and filter the polyamide-imide powder. Place the filtered polyamide-imide powder in a soap solution with the same components as in Step 1 for washing. After washing, dry in a hot air drying oven at 90°C for 12 hours.

[0063] Example 6

[0064] Step 1: Weigh 60g of purified water and 0.18g of laundry detergent at room temperature to prepare a soaping solution with a concentration of 3g / L. Add 2g of polyamide-imide powder to the soaping solution and soap for 15 minutes at a soaping temperature of 70℃. After soaping, dry in a hot air drying oven at 70℃ for 12 hours.

[0065] Step 2: Prepare the dye solution. Add 0.08g of cationic red dye, 60g of purified water, and 1.6g of benzyl alcohol to a beaker. Adjust the pH of the dye solution to 4-5 using acetic acid. Stir the dye solution continuously for 30 minutes to ensure uniformity. The dye solution is now ready. Mix the dried powder into the prepared dye solution, place the mixture in a constant temperature magnetic stirring oil bath with a magnetic stir bar, and slowly heat to 130℃. Maintain this temperature for 60 minutes while continuously stirring.

[0066] Step 3: Stop heating and continue stirring until it slowly cools to room temperature. Rinse and filter the polyamide-imide powder. Place the filtered polyamide-imide powder in a soap solution with the same components as in Step 1 for washing. After washing, dry in a hot air drying oven at 90°C for 12 hours.

[0067] The staining rates of the samples after staining in Examples 1-6 above are shown in Table 1:

[0068] Table 1. Staining rates of different examples

[0069]

[0070] Figure 2 The images show the UV absorption spectra of the original dye solution and the dye solutions used in Examples 1 to 6 after dyeing, after dilution, at 400nm-600nm. The dilution ratio was 115 times. According to the formula... The dyeing rates were calculated (where A0 is the absorbance at the maximum absorption wavelength after the dye solution is diluted n times before dyeing, and A1 is the absorbance at the maximum absorption wavelength after the dye solution is diluted m times after dyeing), and the results are shown in Table 1. The UV test results from Examples 1 to 6 show that increasing the benzyl alcohol content significantly affects the dyeing rate (under the same conditions, the dyeing rate is approximately 40% without a dyeing carrier), indicating that the addition of benzyl alcohol carrier can improve the dyeing rate of polyamide-imide powder, allowing it to combine with more dye and achieve the desired dyeing effect. Simultaneously, different pH values ​​also have a certain impact on the dyeing rate; the dyeing effect is optimal at a pH of 4-5.

[0071] Infrared spectroscopy of undyed polyamide-imide powder and powder after dyeing in Example 6 are as follows: Figure 3 As shown, they all possess structures such as imide, amide, methylene, and benzene ring. A change in the intensity of the vibrational absorption peak of the benzene ring skeleton was observed after staining, and it reached 1780... -1 1660 -1 The characteristic peak at 1375 decreased. -1 and 1720 -1 The peak gradually shifted towards 1373. -1 and 1718 -1 The results showed that after staining, the surface of the PAI structure underwent slight hydrolysis, but the molecular structure of the polyamide imide was not affected.

[0072] Example 6: Thermogravimetric analysis after staining. Figure 4 As shown, from Figure 4 It can be seen that the polyamide-imide powder treated with carrier dyeing at 130℃ remains stable up to 400℃ (the weight loss at 170℃ corresponds to the weight loss of incompletely dried water and aprotic polar solvent). Significant weight loss occurs when the gas temperature reaches approximately 527℃, and the weight loss rate reaches 44.18% when the temperature reaches the set maximum of 800℃. The figure illustrates that the thermal stability of polyamide-imide after dyeing using this method is not significantly affected, and it still maintains excellent thermal stability.

[0073] Five different colored polyamide-imide powders were synthesized using the staining method proposed in Example 6 and different cationic dyes. The UV absorption spectra of the dye solutions after staining the five colored samples, after being diluted by the same factor, at 400 nm-600 nm are shown below. Figures 5 to 9 As shown ( Figures 5 to 9The optimal dyeing rate parameters obtained by the cationic dyeing method based on polyamide-imide powder in this invention (using benzyl alcohol as a carrier, and measuring the UV absorbance of samples stained with different types of cationic dyes) all showed a dyeing rate of over 70%. Figure 5 For the black sample, cationic black CX-2GL was used; Figure 6 For the brown sample, cationic black XO was used; Figure 7 For the green sample, cationic blue X-BL and cationic yellow X-8GL were used; Figure 8 For blue samples, cationic blue X-BL was used; Figure 9 For the purple sample, cationic brilliant violet X-5BLH was used.

Claims

1. A cationic dyeing process based on polyamide-imide powder, characterized in that: Specifically comprising the following steps: Step 1, pretreatment of polyamide-imide powder; the specific process of step 1 is: put the polyamide-imide powder into the soaping solution for soaping, dry after washing; Step 2, put the polyamide-imide powder treated in step 1 into the dyeing solution for dyeing, put the dyed polyamide-imide powder into the soaping solution containing washing powder solution for soaping to remove the residual dye and oil stains on the surface of the fabric, dry after washing to obtain; The specific process of step 2 is: Step 2.1, put the polyamide-imide powder treated in step 1 into the dyeing solution, heat at a rate of 2℃ / min, the dyeing temperature is 80-140℃, then keep warm for 60min; in step 2.1, the preparation process of the dyeing solution is: Add cationic dye, purified water and benzyl alcohol in a beaker, adjust the pH of the solution to 3-6, and stir uniformly to obtain the prepared dyeing solution; Step 2.2, stop heating and continue stirring until the temperature of the dyeing solution cools to room temperature, then wash and dry, put the dyed polyamide-imide powder into the soaping solution for soaping, dry after soaping.

2. The cationic dyeing method based on polyamide-imide powder according to claim 1, characterized in that: In step 1, the amount of polyamide-imide powder is 1-20g, the concentration of washing powder in the soaping solution is 1-3g / L, the soaping temperature is 50-90℃, the soaping time is 10-20min; the drying temperature is 60-80℃, and the drying time is 8-16h.

3. The cationic dyeing method based on polyamide-imide powder according to claim 1, characterized in that: In step 2.1, the mass ratio of polyamide-imide powder to dyeing solution is 1:15-30; the mass of cationic dye is 1-5% of the mass of polyamide-imide powder, and the concentration of benzyl alcohol is 10-60g / L.

4. The cationic dyeing method based on polyamide-imide powder according to claim 3, characterized in that: In step 2.2, the concentration of washing powder in the soaping solution is 1-3g / L, the mass of the soaping solution is 30 times the mass of the powder used, the soaping temperature is 50-90℃, and the soaping time is 10-20min.

5. The cationic dyeing method based on polyamide-imide powder according to claim 4, characterized in that: In step 2.2, the drying temperature after dyeing is 80-120℃, and the drying time is 8-16 hours.

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